HRID490475

反应详情

EQUATION

反应方程式

HRID 490475 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
3 °C

PROCEDURE

实验过程

A solution of 5-benzyltetrahydropyrrolo[3,4-c]pyrrole-1,3-dione, (12.7 g; 55 mmol) {preparation described for the preparation of cis-perhydropyrrolo[3,4-c]pyrrole-1,3-dione (b)} is added to a suspension of lithium aluminum tetrahydride (2 g; 55 mmol) in tetrahydrofuran, cooled to 3° C. in an ice bath, in a 500 ml three-necked flask. The reaction mixture is agitated at this temperature for 25 minutes and then water (2 ml), 4 N aqueous sodium hydroxide (2 ml) and water (6 ml) are successively added. The solid thus formed is removed by filtration; the filtrate is dried over magnesium sulfate and then evaporated under reduced pressure, resulting in a white solid which is triturated in diisopropyl ether (50 ml). The solid formed is filtered off, washed with diisopropyl ether (25 ml), and then dried under reduced pressure at constant weight. 5-Benzyl-3-hydroxyhexahydropyrrolo[3,4-c]pyrrol-1-one (7 g; 55%) is isolated, the characteristics of which are as follows:

WORKUP

后处理

  1. customThe solid thus formed
  2. customis removed by filtration
  3. dry with materialthe filtrate is dried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. customresulting in a white solid which
  6. customis triturated in diisopropyl ether (50 ml)
  7. customThe solid formed
  8. filtrationis filtered off
  9. washwashed with diisopropyl ether (25 ml)
  10. customdried under reduced pressure at constant weight