Amides-buliding-blocks

Some common heterocyclic compound, 37073-15-7, name is 1-(Methylsulfonyl)-1H-benzo[d][1,2,3]triazole, molecular formula is C7H7N3O2S, 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. Computed Properties of C7H7N3O2S

Example 1 (E)-1-(benzotriazol-1-yl)-3-phenyl-2-propen-1-one 1.42 g (0.01 mol) of trans-cinnamic acid (compound of formula IV) and 1.97 g (0.01 mol) of 1-(methylsulfonyl)benzotriazole are stirred at room temperature in 50 ml of tetrahydrofuran, followed by dropwise addition of 0.014 mol of triethylamine. The solution is then refluxed for 24 hours, and then evaporated under reduced pressure. The residue is taken up in 60 ml of water and extracted with 70 ml of ethyl acetate. The organic phase is dried, filtered and then concentrated under vacuum. The powder obtained is taken up in 50 ml of acetonitrile and filtered off by suction. 2.24 g of a white powder are obtained. Melting point: 157 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 37073-15-7, its application will become more common.

Reference:
Patent; PRODUITS CHIMIQUES AUXILIAIRES ET DE SYNTHESE; Rault, Sylvain; Lancelot, Jean Charles; Suzanne, Peggy; Voisin-Chiret, Anne-Sophie; Pecquet, Regis; Joseph, Jean-Christophe; US2013/165507; (2013); A1;,
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Synthetic Route of 94838-59-2, 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 94838-59-2 as follows.

A mixture of 2-(3-bromopropoxy)tetrahydro-2//-pyran (669mg,3 mmol), tert- butyl 4- aminophenethylcarbamate (709 mg, 3 mmol) and cesium carbonate (2.9 g, 9 mmol) in DMF (20 mL) was stirred at 110 C for 2 h. TLC showed the reaction completed. The reaction mixture was filtered. The filtrate was concentrated and purified by column chromatography to afford the title compound as yellow oil (l80mg, 15.9% yield). NMR (500 MHz, DMSO-r/6) S: 6.94 (d, J= 8.3 Hz, 2H), 6.84 (t, J= 5.4 Hz, 1H), 6.54 (d, J= 8.4 Hz, 2H), 5.42 (t, J= 5.6 Hz, 1H), 4.61 (t, J= 3.4 Hz, 1H), 3.79 (tt, J= 12.6, 4.8 Hz, 2H), 3.49 (dt, J= 9.4, 6.2 Hz, 2H), 3.16 – 3.02 (m, 4H), 2.58 (d, J= 8.0 Hz, 2H), 1.87 – 1.64 (m, 4H), 1.57 – 1.47 (m, 4H), 1.41 (d, J= 15.5 Hz, 9H).

According to the analysis of related databases, 94838-59-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ZHEJIANG VIMGREEN PHARMACEUTICALS, LTD; SUN, Sanxing; ZHAO, Long; HU, Chongbo; CHEN, Zhengshu; YE, Jinqi; (0 pag.)WO2020/2969; (2020); A1;,
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Synthetic Route of 125414-41-7, 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. 125414-41-7, name is tert-Butyl (1,3-dihydroxypropan-2-yl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

tert-Butyl (l,3-dihydroxypropan-2-yl)carbamate (3.7 g, 19.35 mmol), potassium hydroxide (4.0 g, 71.59 mmol), and benzyl bromide (12.24 g, 71.59 mmol) were dissolved in 50 mL of DMF. The mixture was stirred for 2 h and concentrated under vacuum. The crude product was purified using column chromatography to yield tert-butyl (1 ,3-bis(benzyloxy)propan-2- yl)carbamate (3.25 g, 45% yield).

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 (1,3-dihydroxypropan-2-yl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NEKTAR THERAPEUTICS (INDIA) PVT.LTD.; NEKTAR THERAPEUTICS (Incorporated under the Laws of Delaware and domiclled in the State of California); DUARTE, FRANCO; ANAND, NEEL; SHARMA, PANKAJ; SINGH, DEVENDRAPRATAP U.; WO2015/79459; (2015); A1;,
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Reference of 326-67-0,Some common heterocyclic compound, 326-67-0, name is N-(2-Fluoro-4-methylphenyl)acetamide, molecular formula is C9H10FNO, 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.

To 546 g (3.27 mol) of crude 2-fluoro-4-methyl-acetanilide was added chlorosul- phonic acid (2000 g, 17.24 mol) with stirring at a temperature below 70C. Stirring was continued for 3 hours at a temperature of 70C. The reaction mixture was poured onto ice and then extracted with ethyl acetate. The organic phase was dried with sodium sulfate and concentrated under reduced pressure to yield the title compound (500 g, 57.8%). H NMR (400 MHz, CDCI3): delta = 9.1 (d, 1 H, J = 7.2 Hz), 7.39-7.52 (m, 1 H), 7.14 (d, 1 H, J = 1 1 .2 Hz), 2.72-2.78 (m, 3H), 2.2-2.3 (m, 3H).

The synthetic route of 326-67-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; KAISER, Florian; GROss, Steffen; LANGEWALD, Juergen; NARINE, Arun; WO2013/30262; (2013); A1;,
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Electric Literature of 201162-53-0,Some common heterocyclic compound, 201162-53-0, name is 3-Boc-3,8-Diazabicyclo[3.2.1]octane, molecular formula is C11H20N2O2, 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.

3,8-diazabicyclo [3.2.1] octane-3-carboxylic acid tert-butyl ester (320 mg, 1.5 mmol)And bromoethane (817 mg, 7.5 mmol)Was dissolved in acetonitrile (50 mL), potassium carbonate (1.03 mg, 7.5 mmol) was added and reacted at 40 C for 16 hours.The organic phase was combined, washed with saturated brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound which was extracted with ethyl acetate (50 mL) The title compound was obtained as a color oil (350 mg, yield 97%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Boc-3,8-Diazabicyclo[3.2.1]octane, its application will become more common.

Reference:
Patent; Shandong Xuanzhu Pharmaceutical Technology Co., Ltd.; Wu, Yongqian; (45 pag.)CN104910137; (2017); B;,
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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. 85006-25-3, name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate, A new synthetic method of this compound is introduced below., name: tert-Butyl (tert-butoxycarbonyl)oxycarbamate

Example 17: 7¾ -butyl i2-fl2-amino-3-chloro-6,7,10,ll-tetrahydro-7,ll- methano cvcloocta[bl uinolin-9-yl)ethyll (tert- butox carbonvDoxyl carbamate (HUP 16)A solution of tert-butyl-N-(tert-butoxycarbonyl)-carbamate (140 mg, 0.6 mmol) in anhydrous DMF (1.3 mL) was treated with sodium hydride (60% in oil, 26 mg, 0.65 mmol). The reaction mixture was stirred 40 min at r.t. and treated with a solution of mesylate (HUP 13) (157 mg, 0.4 mmol) in anhydrous DMF (2 mL). The reaction mixture was stirred at r.t. for 120 h, then at 60 C for 5 h. The mixture was then diluted with water (50 mL) and extracted with AcOEt (3 x 30 mL). The combined organic layers were washed with brine (50 mL), then water (50 mL), dried with Na2S04 and concentrated under reduced pressure to afford a yellow solid (313 mg). Purification by flash chromatography (AcOEt / MeOH 10/0 to 8/2, v/v) afforded the desired Huprine (HUP 16) as a white solid (98 mg, 46%).Rf (AcOEt / MeOH 8/2, v/v) = 0.50.m.p. = 114C (decomposition).1H NMR (300 MHz, CDC13): delta = 1.41 (s, 9H, N-Boc or O-Boc), 1.46 (s, 9H, N- Boc or O-Boc), 1.84-2.02 (m, 3H, Hio, ¾), 2.10-2.22 (m, 2H, Hi4), 2.52 (dd, J = 17.1 Hz, J = 3.4 Hz, 1H, ¾), 2.67-2.71 (m, 1H, H7), 2.89 (d, J = 17.5 Hz, 1H, H6), 3.06 (dd, J = 17.6 Hz, J = 5.6 Hz, 1H, H6), 3.14-3.18 (m, 1H, Hn), 3.66-3.88 (m, 2H, His), 5.03 (brs, 2H, NH2), 5.56 (d, J = 5.1 Hz, 1H, H8), 7.21 (dd, J = 9.0 Hz, J= 1.9 Hz, 1H, H2), 7.67 (d, J= 9.0 Hz, 1H, ¾), 7.77 (d, J= 1.9 Hz, 1H, H4). 13C NMR (75 MHz, CDC13): delta = 27.4 (Cn), 27.6 (N-Boc or O-Boc), 28.1 (N-Boc or O-Boc), 28.2 (C7), 28.9 (C10), 33.8 (C13), 34.8 (Ci4), 39.4 (C6), 68.1 (Ci5), 82.3 (C-Me3 of N-Boc), 84.9 (C-Me3 of O-Boc), 115.1 (Cna or Ci2a), 115.8 (Cna or Ciza), 122.0 (Ci), 124.6 (C2), 126.9 (C4), 127.0 (C8), 132.9 (C3), 134.6 (C9), 146.5 (C4a or Ci2), 147.0 (C4a or C12), 152.2 (C=0 of N-Boc), 154.8 (C=0 of O-Boc), 158.3 (C5a).MS (ESI+): m/z (%): 530.20 (100) [M+H]+, 532.20 (39).ICso rh-AC E : 14.8 +/- 3.2 nM.ICso r/i-BuChE : 421 +/- 72 nM.

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:
Patent; UNIVERSITE DE ROUEN; RONCO, Cyril; RENARD, Pierre Yves; JEAN, Ludovic; NACHON, Florian; ROMIEU, Anthony; WO2011/124712; (2011); A1;,
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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. 4424-80-0, name is 4,5-Dihydro-1H-benzo[b]azepin-2(3H)-one belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 4424-80-0

To a mixture of 4,5-dihydro-lH-benzo[b]azepin-2(3H)-one (10.6 g, 65.8 mmol) in DCM (150 mL) cooled in an ice/water bath was added TMEDA (29.8 mL, 197 mmol), then dropwise over 20 minutes was added TMSI (26.9 mL, 197 mmol). The mixture was stirred cooled for 60 minutes, iodine (25.03 g, 99 mmol) was added and the mixture was stirred cooled for another 60 minutes. The reaction was quenched with 5% Na2S2C”3 and stirred 15 minutes. The resulting solid was filtered and dried to give 11.3 g tan solid. Layers of filtrate were separated. Organics were concentrated to a solid, triturated in diethyl ether and solid was filtered and dried to give 5.52 g light brown solid (87% yield, both batches). 1H MR (DMSO-de) delta: 9.93 (s, 1H), 7.22 – 7.30 (m, 2H), 7.09 – 7.17 (m, 1H), 6.99 (d, J = 7.3 Hz, 1H), 4.63 (dd, J = 9.1, 6.8 Hz, 1H), 2.52 – 2.81 (m, 4H); MS (m/z) 288.0 (M+H+).

The synthetic route of 4424-80-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BANDYOPADHYAY, Deepak; EIDAM, Patrick M.; GOUGH, Peter J.; HARRIS, Philip Anthony; JEONG, Jae U.; KANG, Jianxing; KING, Bryan Wayne; LAKDAWALA SHAH, Ami; MARQUIS, JR., Robert W.; LEISTER, Lara Kathryn; RAHMAN, Attiq; RAMANJULU, Joshi M.; SEHON, Clark A; SINGHAUS, JR., Robert; ZHANG, Daohua; WO2014/125444; (2014); A1;,
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Electric Literature of 609-66-5, 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 609-66-5 as follows.

General procedure: An oven-dried Schlenk tube was charged with benzamide 1 (0.5 mmol), K2CO3 (207 mg, 1.5 mmol) and aryl iodide 2 (1.0 mol). The tube was evacuated and backfilled with N2 (3 ×), and then DMEDA (0.2 mmol) and anhyd toluene (5.0 mL) were added. The reaction mixture was stirred at 110 C for 48 h. H2O was added and the crude product was extracted with EtOAc. The combined organic phases were washed with brine and H2O, dried (Na2SO4), and concentrated under reduced pressure. The product was purified by silica gel chromatographyto give the desired N-arylated benzamides (Table 2).

According to the analysis of related databases, 609-66-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Huang, Fei; Wu, San; Hu, Weiye; Zhang, Songlin; Synthesis; vol. 50; 5; (2018); p. 1090 – 1096;,
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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. 563-83-7, name is Isobutyramide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of Isobutyramide

A solution containing isobutyramide (10 g, 115 mmol) in THF (250 mL) was treated with phosphorous pentasulfide (4.1 g, 9.22 mmol), stirred at 25 C. for 64 hours, concentrated and partitioned between ethyl acetate and water. The organic phase was washed with brine and dried over MgSO4, filtered and concentrated to give the title compound (8.6 g, 73% yield), which was used without further purification.

The synthetic route of 563-83-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DeGoey, David A.; Flentge, Charles A.; Flosi, William J.; Grampovnik, David J.; Kempf, Dale J.; Klein, Larry L.; US2005/131017; (2005); A1;,
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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 125414-41-7 as follows. HPLC of Formula: C8H17NO4

The suspension of powdered KOH (3.05 g) and anhydrous THF (15 mL) was cooled to 0 C, Ar protection. Compound 2 (2.06 g) was dissolved in dry THF (10 mL) Was added dropwise to the reaction solution, After adding 0 reaction 15min, A solution of 4.7 mL of bromopropyne was added dropwise, 0 reaction 5min after the temperature to 35 C overnight, Deionized water (100 mL) was added, CH2Cl2 extraction, Saturated brine washing, Anhydrous Na2SO4 dried, filter, concentrate, Column separation, A yellow liquid 3 (2.467 g, 88%) was obtained.

According to the analysis of related databases, 125414-41-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangxi University; Wang, Mian; Wang, Jianyi; Chen, Zhengjun; (18 pag.)CN106554378; (2017); A;,
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