1,3-DiMethyl 2-[4-(Methoxycarbonyl)-2-nitrophenyl]propanedioate synthesis
- Product Name:1,3-DiMethyl 2-[4-(Methoxycarbonyl)-2-nitrophenyl]propanedioate
- CAS Number:1160293-27-5
- Molecular formula:C13H13NO8
- Molecular Weight:311.24
14719-83-6
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Yield: 95.4%
Reaction Conditions:
with sodium tert-pentoxide in 1-methyl-pyrrolidin-2-one at 75; for 1.5 h;
Steps:
1
Synthesis of propanedioic acid, [4-(methoxycarbonyl)-2-nitrophenyl]-, dimethylester12,87kg of malonic acid, dimethylester (97,41 mol) is added to a hot solution (75°C) of 10,73kg sodium-tert.amylate (97,41 mol) in 35L 1 - methyl-2-pyrrolidinone (NMP). A solution of 10kg benzoic acid, 4-chloro- 3-nitro-, methylester (46,38mol) in 25L 1 -methyl-2-pyrrolidinone is added at 75°C. After stirring for 1.5 hours at about 75°C and cooling to 20°C, the mixture is acidified with 100L diluted hydrochloric acid to pH 1. After stirring for 1.5 hours at about 5°C, the product is isolated by centhfugation and drying at 40°C. Yield: 13,78kg (95,4% of theoretical amount) Purity (HPLC): 99,9%
References:
BOEHRINGER INGELHEIM INTERNATIONAL GMBH WO2009/71524, 2009, A2 Location in patent:Page/Page column 15; 5
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