HRID1618636

反应详情

EQUATION

反应方程式

HRID 1618636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-bromo-1H-indole-3-carbaldehyde (1.2 g, 5.36 mmol) in pyridine (10 mL) was added NH2OH.HCl (0.424 g, 6.11 mmol) portionwise and the resulting mixture was stirred at rt for 1.5 h. 25 mL of Ac2O was added and the mixture was heated at reflux overnight. After this time the reaction mixture was cooled to rt and poured into ice. The resulting solid was filtered and the product was purified by flash column chromatography to give 6-bromo-1H-indole-3-carbonitrile slightly impure but was used for the next step. Mass Spectrum (ESI) m/e=222 (M+1).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux overnight
  3. temperatureAfter this time the reaction mixture was cooled to rt
  4. additionpoured into ice
  5. filtrationThe resulting solid was filtered
  6. customthe product was purified by flash column chromatography