1H-BenziMidazole-2-carboxylic acid, 5-nitro-, Methyl ester synthesis
- Product Name:1H-BenziMidazole-2-carboxylic acid, 5-nitro-, Methyl ester
- CAS Number:93521-65-4
- Molecular formula:C9H7N3O4
- Molecular Weight:221.17
Yield:93521-65-4 91%
Reaction Conditions:
Stage #1: methanol;5-nitro-2-(trichloromethyl)-1H-benzo[d]imidazolewith sodium carbonate for 4 h;Reflux;
Stage #2: with sodium hydrogencarbonate for 4 h;Reflux;
Steps:
2.2 Methyl 5-nitro-1H-benzo[d]imidazole-2-carboxylate
5-Nitro-2-(trichloromethyl)-1H-benzo[d]imidazole 2b (5g, 17.83mmol) and sodium carbonate (2.89g, 29.83mmol) were suspended in 200mL of methanol.
The reaction solution was heated to reflux for 4 hours, then sodium bicarbonate (1g, 12mmol) was added, the mixture was heated to reflux continuously for 4 hours.
The reaction solution was concentrated under reduced pressure, 1M hydrochloric acid was added to the residue, solid precipitated, the residue was subjected to suction filtration, the filter cake was washed with water (20mL*5) and then subjected to infrared drying to obtain methyl 5-nitro-1H-benzo[d]imidazole-2-carboxylate 2c (3.6g, brown solid), yield: 91%.
MS m / z (ESI): 221.9 [M + 1]
References:
EP3339305,2018,A1 Location in patent:Paragraph 0078; 0080
99-56-9
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