HRID1894740

反应详情

EQUATION

反应方程式

HRID 1894740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-nitroso-2,3-dihydro-1H-indole (5.27 g, 35.6 mmol) in tetrahydrofuran (35 ml) was added dropwise to a refluxing slurry of lithium aluminium hydride (2.98 g, 78.5 mmol) in tetrahydrofuran (100 ml). After 1 hour the mixture was cooled in an ice bath and water (3 ml) carefully added. 2M sodium hydroxide (6 ml) followed by water (6 ml) were added and the mixture heated to reflux for 30 minutes. After cooling to room temperature the precipitate formed was filtered off. The filtrate obtained was evaporated to dryness to yield 2,3-dihydro-indol-1-ylamine as a red/brown oil (4.216 g), which was used for the next step without further purification.

WORKUP

后处理

  1. temperatureAfter 1 hour the mixture was cooled in an ice bath
  2. additionwere added
  3. temperaturethe mixture heated
  4. temperatureto reflux for 30 minutes
  5. customformed
  6. filtrationwas filtered off
  7. customThe filtrate obtained
  8. customwas evaporated to dryness