Month: January 2021

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 22503-72-6 as follows. Product Details of 22503-72-6

To an ice-cooled solution of 1 (233 mg, 1.0 mmol) in CH2Cl2 (10mL) was added dropwise an excess of MCPBA (1478 mg, 6.0mmol, 70%) in CH2Cl2 (10 mL) previously cooled in an ice bath.The mixture was allowed to gradually warm to r.t., with stirring,over 12 h. TLC and LC-MS analyses were used to monitor reactionprogress. When the reaction was complete, the solution was stirredwith excess powered anhydrous Na2CO3 until carbon dioxide evolutionceased. After filtration, the mixture was concentrated in vacuoat r.t. to give pure 2.Yield: 275 mg (99%); yellow solid; mp 160-163 C.IR (KBr): 3160, 3101, 2990, 1600, 1550, 1350, 850 cm-1.1H NMR (400.13 MHz, CDCl3): delta = 2.48 (s, 3 H, CH3), 7.63 (d,J = 9.0 Hz, 1 H, ArH), 7.98 (d, J = 9.0 Hz, 1 H, ArH), 8.06 (s, 1 H,ArH), 9.25 (br s, 1 H, NH).13C NMR (100.62 MHz, CDCl3): delta = 16.8, 125.4, 126.9, 133.0,135.8, 138.1, 143.5, 165.7.HRMS (ESI): m/z [M + H]+ calcd for C8H7ClN2O5S: 278.9842;found: 278.9840.

According to the analysis of related databases, 22503-72-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Cannazza, Giuseppe; Perrone, Serena; Rosato, Francesca; D’Accolti, Lucia; Parenti, Carlo; Troisi, Luigino; Synthesis; vol. 46; 7; (2014); p. 962 – 966;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 869494-16-6, name is tert-Butyl 3,6-diazabicyclo[3.1.1]heptane-6-carboxylate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of tert-Butyl 3,6-diazabicyclo[3.1.1]heptane-6-carboxylate

A mixture of 1-bromo-4-iodobenzene (0.500 g, 1.77 mmol), tert-butyl 3,6- diazabicyclo[3.1.1]heptane-6-carboxylate (0.491 g, 2.47 mmol), C52CO3(s) (1.15 g, 3.53 mmol), CuT (16.8 mg, 0.0884 mmol) and 2-isobutyrylcyclohexan-1-one (59.5 mg, 0.353 mmol) in DMF (1.5 mL) was sparged with Ar(g) for 5 mm, then stirred for 4 days at ambient temperature. The reaction mixture was treated with additional CuT (16.8 mg, 0.0884 mmol), then sparged with Ar(g) for 5 mm and stirred at 35 ¡ãC for 1 h. The mixture was partitioned between brine and MTBE. The organic layer was separated and washed with additional brine and saturated NH4C1(aq). The aqueous extracts were combined and back extracted with MTBE. The MTBE extracts were combined, then dried over anhydrous MgSO4(), filtered, and concentrated in vacuo. The crude residue was purified by silica chromatography (DCM as the eluent) to cleanly provide the title compound (190 mg, 30percent yield). MS (apci) m/z = 353.0 (M+1); 355.1 (M+2) with Br pattern.

The synthetic route of 869494-16-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ANDREWS, Steven W.; ARONOW, Sean; BLAKE, James F.; BRANDHUBER, Barbara J.; COOK, Adam; HAAS, Julia; JIANG, Yutong; KOLAKOWSKI, Gabrielle R.; MCFADDIN, Elizabeth A.; MCKENNEY, Megan L.; MCNULTY, Oren T.; METCALF, Andrew T.; MORENO, David A.; TANG, Tony P.; REN, Li; (668 pag.)WO2018/71447; (2018); A1;,
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These common heterocyclic compound, 112253-70-0, name is 2-Amino-4-bromobenzamide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 2-Amino-4-bromobenzamide

PR-9 QA-4 Oxalyl dichloride (2.5 mL, 13.11 mmol) was added drop wise to a mixture of the compound PR-9 (2.5 g, 8.74 mmol), 2-amino-4-bromobenzamide (2.5 g, 10.49 mmol) in dichloromethane (20 mL) and pyridine (20 mL) at room temperature. The mixture was stirred for 1 hour at room temperature. The solvent was removed in vacuo. The residue was purified by column chromatography (petroleum ether: acetate ether=l : 1) . The obtained intermediate amide compound (0.98 g), Na2C03 (1.08 g. 10.15 mmol), H20 (5 mL) and CH3CH2OH (5 mL) were stirred for 2 hours under reflux. Most of CH3CH2OH was removed in vacuo and the obtained residue was extracted with ethyl acetate. The organic layer was dried over Na2S04 and concentrated in vacuo. The residue was washed with t-butyl methyl ether resulting in compound QA-4 (0.89 g).

The synthetic route of 2-Amino-4-bromobenzamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN R&D IRELAND; VANDYCK, Koen; VERSCHUEREN, Wim, Gaston; RABOISSON, Pierre, Jean-Marie, Bernard; WO2013/98313; (2013); A1;,
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Some common heterocyclic compound, 71026-66-9, name is tert-Butyl (4-aminophenyl)carbamate, molecular formula is C11H16N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. HPLC of Formula: C11H16N2O2

General procedure: Mucohalic acid (1 eq) was added to a solution of 5:3 v/v dichloromethane/glacial acetic acid. Then, an amine (1 eq) was added, and the mixture was stirred for 10 min. To that mixture, sodium triacetoxyborohydride (3 eq) solution in 5:3 v/v dichloromethane and glacial acetic acid was added. The mixture was left to stir at room temperature for 24 h unless otherwise stated.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 71026-66-9, its application will become more common.

Reference:
Article; Almohaywi, Basmah; Taunk, Aditi; Wenholz, Daniel S.; Nizalapur, Shashidhar; Biswas, Nripendra N.; Ho, Kitty K. K.; Rice, Scott A.; Iskander, George; Black, David StC.; Griffith, Renate; Kumar, Naresh; Molecules; vol. 23; 5; (2018);,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 4141-08-6, name is 2-Amino-N-methylbenzamide, A new synthetic method of this compound is introduced below., SDS of cas: 4141-08-6

General procedure: A flask was charged with 2-aminobenzamide (1a; 27.2 mg, 0.2 mmol), pentane-2,4-dione (2A;30.0 mg, 0.3 mmol), FeCl3¡¤6H2O (10.8 mg, 0.04 mmol), and PEG-400/H2O (1.0 mL, 1:9 (v/v)).The reaction was stirred at 100 C for 24 h. When the reaction was complete monitored by TLC,the mixture was cooled to room temperature, extracted with EtOAc (3¡Á20 mL). The combined organic phase was washed with water, dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the product 3aA (29.3 mg, 91%) as white solid.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Shen, Guanshuo; Zhou, Haifeng; Sui, Yuebo; Liu, Qixing; Zou, Kun; Tetrahedron Letters; vol. 57; 5; (2016); p. 587 – 590;,
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Adding a certain compound to certain chemical reactions, such as: 148017-28-1, name is tert-Butyl sulfamoylcarbamate, belongs to amides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 148017-28-1, Computed Properties of C5H12N2O4S

(R)-(6-chloro-2,3-dihydrobenzo[b][1,4]dioxin-2-yl)methyl trifluoromethanesulfonate (3 g 9.0 mmol), Boc-sulfamide (1.95 g, 10 mmol), and acetone (45 mL) were placed in a 300 mL round-bottomed flask equipped with a nitrogen inlet and a magnetic stir bar. Potassium carbonate (5 g, 36 mmol) was added to the resulting mixture and stirred for 0.75 h. The progress of reaction was monitored by TLC analysis on silica gel plates using EtOAc/Heptane (1:1) as the eluent. The resulting mixture was filtered to remove the solid carbonate and the filtrate was evaporated under reduced pressure to yield (S)-tert-Butyl (6-chloro-2,3-dihydrobenzo[b][1,4]dioxin-2-yl)methyl(sulfamoyl) carbamate as an oily residue that solidified on standing at room temperature for 24 h.1H NMR (d6-DMSO): delta7.61 (s, 2H), 6.99 (d, J=1.6 Hz, 1H), 6.94-6.86 (m, 2H), 4.49-4.39 (m, 1H), 4.25 (dd, J1=2.3, J2=11.9 Hz, 1H), 4.07 (dd, J1=5.5, J2=11.9 Hz, 1H), 3.92 (dd, J1=7.0, J2=14.9 Hz, 1H), 3.79 (dd, J1=5.5, J2=14.9 Hz, 1H), 1.40 (s, 9H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, tert-Butyl sulfamoylcarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Abdel-Magid, Ahmed; Mehrman, Steven J.; Ferraro, Caterina; US2009/182141; (2009); A1;,
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Related Products of 16091-26-2, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 16091-26-2, name is 3′-Aminobenzanilide, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The solid 5 (0.5 mmol) and quinazoline compound 6 (0.55 mmol) was dissolved in 20 mL of ethyl acetate and 4 mL of DMF. The reaction mixture was stirred for about 48-72 h at 45 oC. The reaction color gradually transformed from pale yellow to orange. The resulting mixture was washed with water (30 mL), dried over Na2SO4, concentrated and purified by flash column chromatography to afford the product 7 (yield 40 to 85%). N-(3-(4-Hydroxy-8-nitroquinazolin-5-ylamino)phenyl)benzamide7a Brown solid; 65% yield, M.p. 264.8-265.3 C IR (KBr): 3419, 2929, 1654, 1597, 1540, 1499, 1454, 1339, 1266, 1098, 890, 829 cm-1; 1H NMR (500 MHz, DMSO-d6): deltappm 6.70-6.72 (d, J = 10 Hz, 1H, ArH), 7.10-7.12 (d, J = 10 Hz, 1H, ArH), 7.25-7.28 (m, 1H, ArH), 7.52-7.56 (m, 3H, ArH), 7.59-7.61 (d, J = 10 Hz, 2H, ArH), 7.94-7.95 (d, J = 5 Hz, 2H, ArH), 8.23-8.24 (d, J = 10 Hz, 1H, ArH), 8.30 (s, 1H, NCH=N), 10.27 (s, 1H, NH), 11.59 (s, 1H, NHC=O), 12.99 (br.s, 1H, OH); 13C NMR (125 MHz, DMSO-d6): deltappm 112.55, 113.55, 115.78, 118.25, 118.53, 129.94, 130.68, 131.59, 133.92, 134.29, 134.74, 137.13, 142.53, 142.99, 150.28, 156.24, 166.48, 167.90; HRMS (TOF ESI-): m/z calcd for C21H15N5O4 [(M-H)-], 400.1051; found, 400.1056

The chemical industry reduces the impact on the environment during synthesis 3′-Aminobenzanilide. I believe this compound will play a more active role in future production and life.

Reference:
Article; Zhao, Yongqiang; Liu, Feifei; He, Guojing; Li, Ke; Zhu, Changcheng; Yu, Wei; Zhang, Conghai; Xie, Mingjin; Lin, Jun; Zhang, Jihong; Jin, Yi; Bioorganic and Medicinal Chemistry Letters; vol. 29; 23; (2019);,
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Application of 1408282-26-7, A common heterocyclic compound, 1408282-26-7, name is 8-Fluoro-4,5-dihydro-1H-azepino[5,4,3-cd]indol-6(3H)-one, molecular formula is C11H9FN2O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

8-Fluoro-4,5-dihydro-lH-azepino[5,4,3-cd]indol-6(3H)-one, (lOg; 49.0 mmol) is suspended at ambient temperature in 1 L reactor in 225 mL of dichloromethane/tetrahydrofuran mixture (1/3). Obtained suspension is cooled to 5C while stirring and THF solution of pyridinium tribromide is added dropwise (17.22 g; 53.9 mmol in 75 mL THF). Obtained suspension is stirred at 5C for 2 hours until conversion is complete. Water (100 mL) is added to obtain clear orange solution. Solution is concentrated under vacuum until crystallization occurs. To obtained suspension 750 mL of saturated Na2C03 is added and suspension is stirred for 1 hour at ambient temperature. Obtained crystals are filtered, washed with water (100 mL) and dried in vacuum oven at 55C for 4 hours to obtain 11.3 g of 2-bromo-8-fluoro-4,5-dihydro-lH-azepino[5,4,3-cd]indol-6(3H)-one.

The synthetic route of 1408282-26-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASSIA CHEMICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; SAMEC, Dijana Skalec; DOGAN, Jasna; BILJAN, Tomislav; SKUGOR, Maja Matanovic; MIHOVILOVIC, Moris; MUNDORFER, Tina; JANTON, Nikolina; TUKSAR, Mihaela; PIPERCIC, Sara Morasi; BAUS, Nea; (104 pag.)WO2018/140377; (2018); A1;,
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Synthetic Route of 111300-06-2, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 111300-06-2, name is tert-Butyl (trans-4-hydroxycyclohexyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of PPh3 (1.17 g, 4.47 mmol) in anhydrous toluene (30 mL) was added di-tertbutylazodicarboxylate (DBAD) (1.03 g, 4.47 mmol) at 0 C., and the reaction mixture was stirred for 15 min, after which compound 37-6 (1.40 g, 3.19 mmol) and compound 41-5-1 (894.05 mg, 4.15 mmol) were added and the resulting mixture was stirred at 60 C. for 12 h, the starting materials disappeared. To the mixture, water (100 mL) was added, and the solution was extracted with EtOAc (100 mL¡Á3). The organic phases were combined, dried over anhydrous Na2SO4, and concentrated to give a crude product which was purified by column chromatography (PE/EtOAc=10/1) to afford compound 43-7 (2.00 g, 89.77%) as white solid. LCMS (ESI) m/z: 636 (M+1).

The chemical industry reduces the impact on the environment during synthesis tert-Butyl (trans-4-hydroxycyclohexyl)carbamate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Hubei Bio-Pharmaceutical Industrial Technological Institute Inc.; Humanwell Healthcare (Group) Co., Ltd.; Wang, Xuehai; Wu, Chengde; Xu, Yong; Shen, Chunli; Li, Li’e; Hu, Guoping; Yue, Yang; Li, Jian; Guo, Diliang; Shi, Nengyang; Huang, Lu; Chen, Shuhui; Tu, Ronghua; Yang, Zhongwen; Zhang, Xuwen; Xiao, Qiang; Tian, Hua; Yu, Yanping; Chen, Hailiang; Sun, Wenjie; He, Zhenyu; Shen, Jie; Yang, Jing; Tang, Jing; Zhou, Wen; Yu, Jing; Zhang, Yi; Liu, Quan; (251 pag.)US2017/313683; (2017); A1;,
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Related Products of 622-46-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 622-46-8, name is Phenyl carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of this phenyl carbamate (188 mg, 0.59 mmol) in toluene (3 ml) were added triethylamine (72 mg, 0.71 mmol) and 3-[4-(2-heptylaminoethyl)piperazin-1-yl]propanol (168 mg, 0.59 mmol) and the mixture was stirred at 80 C. for 3 hours. The reaction solution was diluted with water and extracted with chloroform. The organic layer was washed with water and a saturated sodium chloride solution successively, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (silica gel 15 g, developing solvent; chloroform_methanol=40:1 10:1) to provide 249 mg (yield 83%) of N’-[2,4-bis(methylthio)-6-methyl-3-pyridyl]-N-heptyl-N-[2-[4-(3-hydroxypropyl)piperazin-1-yl]ethyl]urea as colorless oil. The same reaction and treatment as in Example 19 were conducted using this urea compound instead of N’-(2,6-diisopropylphenyl)-N-heptyl-N-[2-[4-(3-hydroxypropy 1)piperazin-1-yl]ethyl]urea, and the resulting compound was converted into its salt with hydrochloride in a conventional manner to provide the desired compound as colorless powdery crystals. Melting point: 208-210 C. IR (KBr) cm-1: 3421, 3258, 1658, 1562, 1494. 1H-NMR (d6-DMSO) delta: 0.87 (3H, t, J=6.8 Hz), 1.21-1.35 (8H, m), 1.50-1.66 (2H, m), 2.28 (2H, quint, J=6.6 Hz), 3.39 (6H, s), 2.45 (3H, s), 2.75-4.01 (18H, m), 6.88 (1H, s), 7.30-7.37 (2H, m), 7.63-7.68 (2H, m), 8.34 (1H, br s). Elementary analysis as: C32H48N6O2S3.2HCl Calculated: C, 53.54; H, 7.02; N, 11.71; S, 13.40; Cl, 9.88. Found: C, 53.35; H, 7.01; N, 11.63; S, 13.37; Cl, 9.88.

The synthetic route of Phenyl carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kowa Company, Ltd.; US6969711; (2005); B2;,
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