HRID536099
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Ethyl 3-[(1H-benzimidazol-2-ylmethyl)amino]-1H-pyrrole-2-carboxylate (0.33 g, 1.16 mmol) was added to CH2Cl2 (3 mL) and methanol was added until clear solution was obtained. The solution was stirred at r.t. for 1 h. Benzoyl isothiocyanate (0.73 mL, 0.46 mmol) was added and after stirring at r.t. for 30 minutes the mixture was concentrated. The residue was dissolved in ammonia (7N in methanol, 7 mL) and the mixture was heated at 80° C. in a sealed steel container for 2 h. After cooling to r.t. the precipated product was filtrated and washed through with methanol, diethyl ether and ethyl acetate, obtaining 0.23 g (66%) of the title compound as a white solid.
WORKUP
后处理
- additionwas added until clear solution
- customwas obtained
- stirringafter stirring at r.t. for 30 minutes the mixture
- concentrationwas concentrated
- dissolutionThe residue was dissolved in ammonia (7N in methanol, 7 mL)
- temperaturethe mixture was heated at 80° C. in a sealed steel container for 2 h
- temperatureAfter cooling to r.t. the precipated product
- filtrationwas filtrated
- washwashed through with methanol, diethyl ether and ethyl acetate