Amides-buliding-blocks

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. 6331-71-1, name is 4-Amino-N,N-dimethylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: amides-buliding-blocks

To a 500 ml three-mouth bottle by adding 200 ml of THF, cooling to 5 C the following add 17.3g (0.46mol, 4 . 0eq) of lithium aluminum hydride, then lower the temperature to the -5 C the following, the three aluminum chloride 3.0g (0.023mol, 0 . 2eq) THF slowly dropwise to the reaction in the solution, stirring for 10 min, temperature at 5 C the following starting to drop plus step amide 19.0g (0.114mol, 1 . 0eq) in 100 ml of solution THF. Added after stirring overnight TLC inspection reaction end, cooling to 0 C the following, starting the dropping water filtration, the filter cake is washed with dichloromethane eluviation, concentrated filtrate, vacuum distillation, to obtain colorless oily liquid 12.0g product. Yield: 71.0%, GC: 99.9%

The synthetic route of 6331-71-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shao Yuan Science and Technology (Shanghai) Co., Ltd.; Wu, Yong; Lei, Ting jun; Qi, Ming; (12 pag.)CN105461659; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 16066-84-5 as follows. Recommanded Product: 16066-84-5

To a solution of tert-butyl-N-methylcarbamate (3.00 g, 22.9 mmol) in THF (50 mL) was added NaH (1 .37 g, 34.3 mmol) in portions at 0 C. The reaction mixture was stirred at 15 C for an hour. Then 81 (5.24 g, 22.9 mmol) in THF (20 mL) was added dropwise. The reaction mixture was stirred at 15 C for 13 h. The reaction was quenched by ice water (10 mL) slowly and then extracted with EtOAc (20 mL x 3). The combined organic phase was washed with brine (10 mL x 2), dried over anhydrous Na2S04, filtered and concentrated in vacuo. The residue was purified via silica gel columnchromatography (petroleum ether/ethyl acetate = 4:1) to give 82 (2.9 g, 45%) as a colorless oil.1H N R (400 MHz, CDCI3) 7.95-7.91 (m, 2H), 7.42-7.38 (m, 2H), 4.45 (s, 2H), 3.91 (s, 3H), 2.85 (s, 3H), 1 .48 (s, 9H). To a solution of 82 (2.8 g , 10 mmol) in THF (20 mL) was added LiAIH4(456 mg , 12.0 mmol) in portions at 0 C. The mixture was stirred at 15 C for 2 hours. The mixture was cooled to 0 C and quenched by saturated solution of potassium sodium tartrate (0.5 mL), the mixture was concentrated in vacuum (40C) to give 83 (1 .8 g, 71 %) as a colorless oil.1H NMR (400 MHz, CDCI3) 7.32-7.29 (m, 2H), 7.27-7.23 (m, 1 H), 7.15-7.14 (m, 1 H), 4.68 (s, 2H), 4.42 (s, 2H), 2.82 (s, 3H), 1 .48 (s, 9H). To a solution of 83 (1 .5 g, 6.0 mmol) in DCM (20 mL) was added A/-Fmoc-(S)-valine (2.23 g, 6.57 mmol), DCC (1 .6 g, 7.8 mmol) and DMAP (73 mg, 0.60 mmol). The mixture was stirred at 15 C for 12 h. Then DCM (10 mL) was added and the organic layer was washed with brine (10 mL x 3), dried over Na2S04and concentrated in vacuum. The residue was purified by column chromatography (petroleum ether/ethyl acetate = 4: 1) to give 84 (1 .8 g, 53%) as a colorless oil.1H NMR (400 MHz, CDCI3) 7.70-7.80 (m, 2H), 7.54-7.62 (m, 2H), 7.35-7.42 (m, 2H), 7.23-7.33 (m, 4H), 7.19 (br s, 2H), 5.34-5.32 (m, 1 H), 5.29-5.14 (m, 2H), 4.43-4.41 (m, 4H), 4.40-4.14 (m, 4H), 2.83 (s, 3H), 2.12-2.23 (m, 1 H), 1 .47 (s, 9H), 0.86 (dd, J – 6.84, 2.87 Hz, 6H). To a solution of 84 (1 .00 g, 1 .75 mmol) in THF (6 mL) was added piperidine (298 mg, 3.50 mmol). The mixture was stirred at 15 C for 12 h . The mixture was concentrated in reduced pressure at 40 C. The residue was purified by column chromatography (petroleum ether/ethyl acetate = 1 :4) to give 85 (400 mg, 65%) as a colorless oil.1H NMR (400 MHz, DMSO-d6) 7.37-7.35 (m, 1 H), 7.34-7.29 (m, 1 H), 7.27-7.22 (m, 1 H), 7.18-7.17 (m, 1 H), 5.16-5.06 (m, 2H), 4.37 (s, 2H), 3.15 (d, J – 4.0 Hz, 1 H), 2.74 (s, 3H), 1 .99-1 .84 (m, 1 H), 1 .42-1 .39 (m, 9H), 0.85 (d , J = 6.8 Hz, 3H), 0.79 (s, J = 6.4 Hz, 3H). To a solution of Acid-04 (164 mg, 0.856 mmol) in DMF (3 mL) was added HATU (390 mg, 1 .03 mmol) and TEA (260 mg, 2.57 mmol). The mixture was stirred at 20 C for 1 h. Then 85 (300 mg, 0.856 mmol) was added in one portion. The mixture was stirred at 20 C for 1 1 h. The reaction was quenched by water (10 mL) slowly at 0 C and then extracted with EtOAc (10 mL x 3). The combined organic phase was washed with brine (10 mL x 1), dried over anhydrous Na2S04, filtered and then HCI/EtOAc (4 M, 4 mL) was added. The mixture was stirred at 20 C for 12 h. The mixture was concentrated in vacuo. The residue was purified by prep. HPLC (column: Luna C18 100 x 30 mm; liquid phase: 0.1 %TFA-ACN; B%: 10%-40%, 12 min). After prep. HPLC, 3N HCI (2 mL) was added before freeze drying. 6-122 (137 mg, 33%) was obtained as an off white solid.1H N R (400 MHz, DMSO-cfe) 9.21 (br s, 2H), 9.03 (s, 1 H), 8.59 (d, J – 8.0 Hz, 1 H), 7.55-7.51 (m, 2H), 7.46-7.45 (m, 2H), 7.35 (d, J – 8.0 Hz, 1 H), 7.24 (d, J – 8.0 Hz, 1 H), 5.19 (s, 2H), 4.97 (s, 2H), 4.37 (t, J – 8.0 Hz 1 H), 4.10 (s, 2H), 2.39 (s, 3H), 2.21 -2.16 (m, 1 H), 0.96 (d, J = 6.0 Hz, 6H); ESI-MS m/z 425 [M+H]+; HPLC purity: 94.93% (220 nm), 87.86% (254 nm).

According to the analysis of related databases, 16066-84-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ANACOR PHARMACEUTICALS, INC.; AKAMA, Tsutomu; CARTER, David Scott; HALLADAY, Jason S.; JACOBS, Robert T.; LIU, Yang; PLATTNER, Jacob J.; ZHANG, Yong-Kang; WITTY, Michael John; (149 pag.)WO2017/195069; (2017); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 621-38-5, name is 3-Bromoacetanilide, 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. Recommanded Product: 3-Bromoacetanilide

General procedure: A mixture of Acetylaniline (0.2 mmol), NCS (0.26 mmol), D-CSA (0.1 mmol) and 1,3-di(1-adamantl)imidazolium tetrafluoroborate (0.01 mmol) in dioxane (1 mL) wasstirred at room temperature (25 oC) under air atmosphere for 24h. The reactionmonitored by GC-MS. When the acetylaniline was consumed completely, the reactionmixture was quenched with saturated aq. NaHCO3 (4 mL). The resulting mixture wasextracted with EtOAc (4 mL x 3). The organic layer was washed with pure water (4ml x 3). The combined organic layer was dried over anhydrous Na2SO4, filtered andthe solvent was removed under reduced pressure to provide the crude product. Thepurification was performed by flash column chromatography on silica gel.

The synthetic route of 3-Bromoacetanilide has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Jie; Xiong, Xiaoyu; Chen, Zenghua; Huang, Jianhui; Synlett; vol. 26; 20; (2015); p. 2831 – 2834;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 147291-66-5, 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. 147291-66-5, name is tert-Butyl 3-aminobenzylcarbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 4-chloro-7,8-dimethoxy-1- [1,2,4] triazolo [4,3-a] quinolizinaminophenyl- [ 4] triazolo [4,3-a] quinoxaline (2 g, 7.18 mmol)And diisopropylethylamine (DIPEA, 2.5 ml, 14.4 mmol),tert-Butyl (3-aminobenzyl) carbamate (2.75 ml, 14.4 mmol) was refluxed with 20 ml of isopropyl alcohol for 18 hours. After completion of the reaction, the reaction mixture was cooled to room temperature, and the resulting solid was filtered and dried under reduced pressure to obtain 2.6 g of the target compound

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 3-aminobenzylcarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Korea Research Institute of Chemical Technology; Lee Gwang-ho; Choi Gil-don; Al Ri-im-ran; (56 pag.)KR2018/106597; (2018); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 621-38-5,Some common heterocyclic compound, 621-38-5, name is 3-Bromoacetanilide, molecular formula is C8H8BrNO, 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.

General procedure: The experimental alkylation procedure is similar to that as described in [18]. A screw top vial, under air, was charged with acetanilide substrate (1.0 mmol), [Cp*Co(CO)I2] (20 mol %, 0.20 mmol,95.2 mg), AgSbF6 (40 mol %, 0.4 mmol, 137.4 mg), NaOAc(40 mol %, 0.4 mmol, 16.4 mg), 3-buten-2-one (1.5 equiv,1.5 mmol, 105 mg) and 1,2-DCE (8.0 mL). The vial was sealed,and the reaction mixture heated to 80 C with stirring for 24 hours. After this period, the solvent was removed under reduced pressure and the crude product purified by column chromatography (ethyl acetate/petroleum ether; 80:20 in most cases). For full characterisation data of all products obtained, see Supporting Information File 1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Bromoacetanilide, its application will become more common.

Reference:
Article; Kenny, Andrew; Pisarello, Alba; Bird, Arron; Chirila, Paula G.; Hamilton, Alex; Whiteoak, Christopher J.; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 2366 – 2374;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 25823-52-3, 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 25823-52-3 as follows.

A mixture of the compound of formula (De), 6,7-dihydro-2H- benzo[6,7]cyclohepta[1 ,2-c]pyridazin-3(5H)-one (4.0 g, 19.3 mmol) and POCI3 (20 ml_) was refluxed for 2 h. After cooling to ambient temperature, the volatiles were evaporated. The residue was poured into a mixture of ice water and sodium bicarbonate, CH2CI2 (200 ml_) was added to dissolve the solid. The layers were separated, and the aqueous layer was extracted with CH2CI2 one more time. The combined organic layers were washed with brine. After being dried (MgSO4), filtered, and concentrated, the compound of formula (Df), 3-chloro-6,7-dihydro-5H- benzo[6,7]cyclohepta[1 ,2-c]pyridazine was obtained as a yellow solid (4.3 g, 99%), 1H NMR (300 MHz, CDCI3) delta: 7.82 (m, 1H), 7.45-7.24 (m, 4H), 2.59-2.51 (m, 4H), 2.27 (quant, J = 6.9 Hz, 2H); LC-MS: purity: 100%; MS (m/e): 231 (MH+).

According to the analysis of related databases, 25823-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RIGEL PHARMACEUTICALS, INC.; SINGH, Rajinder; HECKRODT, Thilo, J.; HOLLAND, Sacha; WO2010/5876; (2010); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 141449-85-6, A common heterocyclic compound, 141449-85-6, name is tert-Butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate, molecular formula is C11H20N2O2, 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.

A solution of compound (17b) (100 mg, 0.27 mmol), tert-butyl Hexahydro-pyrrolo[3,4-c]pyrrole-2-carboxylate (86 mg, 0.40 mmol) and DIPEA (187 muL, 1.08 mmol) in 2 mL of DMSO (2 mL) was stirred for 2 days at 80C. The reaction mixture was concentrated under reduced pressure. The residue was triturated with diethyl ether to afford compound (24a) as a yellow solid (139 mg, 0.25 mmol, 94%). MS m/z ([M+H]+) 548.

The synthetic route of 141449-85-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LABORATOIRE BIODIM; Atamanyuk, Dmytro; Chevreuil, Francis; Faivre, Fabien; Lecointe, Nicolas; Ledoussal, Benoit; Oliveira, Chrystelle; Simon, Christophe; EP2913330; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 317595-54-3, name is tert-Butyl (2-aminocyclohexyl)carbamate, 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. Application In Synthesis of tert-Butyl (2-aminocyclohexyl)carbamate

Step 1 cis-N-tert-Butoxycarbonyl-2-(2-ethoxycarbonyl-6-methoxyquinazolin-4-yl)aminocyclohexylamine A solution of 1.96 g of 4-chloro-2-ethoxycarbonyl-6-methoxyquinazoline in 70 mL of toluene was combined with 1.58 g of cis-2-tert-butoxycarbonylaminocyclohexylamine and 0.74 g of triethylamine, and heated under reflux for 15 hours. After concentrating, the mixture was combined with water, extracted with chloroform, and dried. After the solvent was distilled off, the residue was purified by column chromatography on silica gel (chloroform) to obtain 2.70 g of the desirable compound.

The synthetic route of tert-Butyl (2-aminocyclohexyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Okano, Masahiko; Mori, Kazuya; US2003/119855; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 123986-64-1, 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. 123986-64-1, name is tert-Butyl 4-(hydroxymethyl)benzylcarbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(4-Hydroxymethyl~benzyl)-carbamic acid tert-butyl ester (480 mg, 0.71 mmol) was dissolved in DCM (3 ml_) and cooled to -78 0C (dry ice / acetone). Dess-Martin periodinane (331 mg, 0.78 mmol) was added to the reaction which was allowed to warm to r.t and stir for 3 h. A 1 :1 solution of saturated sodium bicarbonate and sodium sulfite (20 ml_) was added and the reaction mixture stirred vigorously for 15 min. The organic layer was isolated, washed with saturated sodium bicarbonate (10 ml_), dried (Na2SO4) and evaporated to dryness to afford the desired compound (480 mg, 100%). m/z 258 [M++Na]+

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 4-(hydroxymethyl)benzylcarbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CHROMA THERAPEUTICS LTD; WO2006/117549; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 53844-02-3, 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. 53844-02-3, name is Benzyl (2-bromoethyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of benzyl(2-bromoethyl)carbamate 9 (129 mg, 0.5 mmol) and the corresponding Michael acceptor 11 (0.5 mmol) in THF (2.5 mL) at 0 C, was added NaH (60% in mineral oil, 24 mg, 0.6 mmol) portion by portion. The ice bath was removed and the reaction mixture was stirred for 3 h to 3 days (monitored by TLC), was then poured into a saturated NH4Cl solution, and extracted with ethyl acetate (2 25 mL). The organic phase was washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The crude mixture was purified by flash chromatography (cyclohexane/EtOAc: 20/ 80).

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, Benzyl (2-bromoethyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Goermen, Meral; Le Goff, Ronan; Lawson, Ata Martin; Daich, Adam; Comesse, Sebastien; Tetrahedron Letters; vol. 54; 17; (2013); p. 2174 – 2176;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics