HRID1171785

反应详情

EQUATION

反应方程式

HRID 1171785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 precipitated 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

  1. additionwas added until clear solution
  2. customwas obtained
  3. stirringafter stirring at r.t. for 30 minutes the mixture
  4. concentrationwas concentrated
  5. dissolutionThe residue was dissolved in ammonia (7N in methanol, 7 mL)
  6. temperaturethe mixture was heated at 80° C. in a sealed steel container for 2 h
  7. temperatureAfter cooling to r.t. the precipitated product
  8. filtrationwas filtrated
  9. washwashed through with methanol, diethyl ether and ethyl acetate