HRID444170

反应详情

EQUATION

反应方程式

HRID 444170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Heat a mixture of 5.0 gm. of 3-cyano-10,11-dihydro-11-oxodibenzo[b,f][1,4]thiazepin and 4.0 gm. of Raney nickel alloy in 60 ml. of 75% (v/v) aqueous formic acid at reflux for 1.5 hours. Cool to room temperature and filter. Concentrate to small volume and extract with methylene chloride. Wash the extract with water and with 1 N sodium bicarbonate until neutral. Dry the neutral extract over sodium sulfate and concentrate to dryness to obtain the title product.

WORKUP

后处理

  1. temperatureHeat
  2. additiona mixture of 5.0 gm
  3. filtrationfilter
  4. concentrationConcentrate to small volume
  5. extractionextract with methylene chloride
  6. washWash the
  7. extractionextract with water and with 1 N sodium bicarbonate until neutral
  8. customDry the
  9. extractionneutral extract over sodium sulfate
  10. concentrationconcentrate to dryness