429659-01-8,Dabigatran Intermediate ETHYL N-[4-(METHYLAMINO)-3-NITROBENZOYL]-N-PYRIDIN-2-YL-SS-ALANINATE

Payment Type: L/C,T/T
Incoterm: FOB
Min. Order: 1 Kilogram
Delivery Time: 15 Days

Basic Info

Model No.: 429659-01-8

Additional Info

Packaging: AS REQUIRED

Productivity: KGS


Transportation: Air

Place of Origin: CHINA

Supply Ability: 100KG

Certificate: ISO

Product Description

 ETHYL N-[4-(METHYLAMINO)-3-NITROBENZOYL]-N-PYRIDIN-2-YL-SS-ALANINATE is the N-4 step intermediate of dabigatran etexilate CAS number is 429659-01-8, the appearance of orange solid, it has two main synthesis methods. Firstly, use 3-nitro-4-chlorobenzoic acid as the starting material, through four steps reaction to get. This method is cumbersome and complicated to operate, with a lower overall yield, making the method more costly to prepare.Secondly, with p-methylaminobenzoic acid as raw material, obtained after 2 steps reaction. The total yield of this method is 94%, which we think is more reliable. The specific procedure is as follows: 1. Take 30.2 g of p-methylaminobenzoic acid mixed with 280 ml of dichloromethane at room temperature and stir for 1 hour, add 32.2 ml of pyridine, cool to -20 ° C., add 10.76 ml of bromine was slowly dropwise and keep the reaction was continued for 5 hours at low temperature. The reaction was quenched with 50 mL of saturated aqueous sodium thiosulfate and then add 100 mL of ethyl acetate. The organic layer was separated and washed with 300 mL of saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and concentrated under reduced pressure to about 100 mL, 50 mL of n-hexane was added, a solid precipitated, and stirred for 2 h at room temperature. The mixture was filtrated, washed with 50 mL of methylene chloride and dried under vacuum at 50 ° C for 1 hour to give 43 g of the first step product.
2. Mixted 34.4 g of the first step product with 240 mL of dichloromethane at room temperature, and stir for 1 hour and cool to -20 ° C. Add thionyl chloride 12 mL and then add N, N-dimethylformamide about 0.5 mL, the reaction was continued for 4 hours, until naturally rising to room temperature,later adding 29.12 g ethyl 3- (pyridin-2-ylamino) propionate and 41.7 mL triethylamine, the reaction was continued for 6 hours at room temperature, The reaction was quenched with 300 mL of water and the organic layer was separated. The organic phase was washed with 200 mL of saturated aqueous sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure to a total volume of about 100 mL. 50 mL of n-hexane was added to precipitate a solid. The mixture was stirred at room temperature for 2.5 hours , Suction filtration,   vacuum dried for 1 hour  at 50 ° C  to give the target compound dabigatran etexilate intermediate CAS number 429659-01-8, ETHYL N-[4-(METHYLAMINO)-3-NITROBENZOYL]-N-PYRIDIN-2-YL-SS-ALANINATE.

Thera. Category: Antithrombotic/Blood thinners

Cas No.:429659-01-8

Synonym:β-Alanine, N-[4-(MethylaMino)-3-nitrobenzoyl]-N-2-pyridinyl-, ethyl ester;ethyl 3-{1-[4-(MethylaMino)-3-nitrophenyl]-N-(pyridin-2-yl)forMaMido}propanoate;N-[4-(MethylaMino)-3-nitrobenzoyl]-N-2-pyridinyl-, ethyl ester Alanine;ETHYL N-[4-(METHYLAMINO)-3-NITROBENZOYL]-N-PYRIDIN-2-YL-SS-ALANINATE;Ethyl 3-(4-(methylamino)-3-nitro-N-(pyridin-2-yl)benzamido)propanoate;Ethyl 3-(4-(ethylaMino)-3-nitro-N-(pyridin-2-yl)benzaMido)propanoate;N-[4-(MethylaMino)-3-nitrobenzoyl]-N-2-pyridinyl-alanine ethyl ester;Ethyl 3-[[4-(MethylaMino)-3-nitrobenzoyl](pyridin-2-yl)aMino]propanoate;


Molecular Weight:386.406

Molecular formula:C19H22N4O5

Purity: ≥99.%

Appearance: White Crystalline solid

Packing:Export worthy packing

Material Safety Data Sheet:Available on request

Usage: It can treat and prevent blood clots, reducing the risk of stroke.

Related intermediate:

Chemical Name Specification Color
41263-74-5 4-(MethylaMino)-3-nitrobenzoic acid HPLC 99.0% pale brown
           103041-38-9 N-[2]PYRIDYL-B-ALANIN-ETHYL ESTER HPLC 99.0% off white to white
           429659-01-8 ETHYL N-[4-(METHYLAMINO)-3-NITROBENZOYL]-N-PYRIDIN-2-YL-SS-ALANINATE HPLC 99.0% orange yellow solid 
N-(4-CYANO-PHENYL)-GLYCINE HPLC 99.0%  off white  
Loss on drying 1.0%
Melting point 101.0°C~106.0°C
Single impurity 0.3% 
Loss on drying 0.5%
Residue on ignition 0.5% 
Assay 98.0%
Synonyms:3-[[[2-[[(4-Cyanophenyl)amino]methyl]-1-methyl-1H-benzimidazol-5-yl]carbonyl]pyridin-2-ylamino]propionic acid ethyl ester HPLC 99.0% off white  
Single impurity 0.3%
Loss on drying 0.5% 
Residue on ignition 0.5% 
Assay 99.0%
 872728-85-3 N-[[2-[[[4-(Aminoiminomethyl)phenyl]amino]methyl]-1-methyl-1H-benzimidazol-5-yl]arbonyl]-N-2-pyridinyl-beta-alanine ethyl ester 4-methylbenzenesulfonate HPLC 97.0% off white  
Dabigatran Etexilate HPLC 98.0%  white  
Single impurity 0.2%
Loss on drying 1.0% 
Assay 98.0%
Dabigatran etexilate mesylate HPLC 99.0%  light yellow solid
Single impurity 0.5%
Loss on drying 1.0% 
Residue on ignition 0.1% 
Heavy melta 20 ppm 
Assay 98.5%

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