HRID2397575

反应详情

EQUATION

反应方程式

HRID 2397575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of lithium aluminum hydride (1 gram, 0.026 mole) in 20 ml dry tetrahydrofuran (THF) is added slowly a suspension of 1,2,3,4-tetrahydro-8-chloro-10-phenylpyrazino[1,2-a] indole-1-one (5.2 grams, 0.018 mole) in 40 ml of dry THF. This reaction mixture is stirred and refluxed for 8 hours after which it is cooled and decomposed by the slow addition of 3 ml of water. After stirring 1 hour the suspension is filtered. The filtercake is washed with isopropanol, THF, and acetone. The combined filtrate is taken to dryness and recrystallized from ethanol. The product is filtered off, washed with ether, and dried. The above titled product has a m.p. 163°-64° C. yield 4.5 grams (90%).

WORKUP

后处理

  1. temperaturerefluxed for 8 hours after which it
  2. temperatureis cooled
  3. stirringAfter stirring 1 hour the suspension
  4. filtrationis filtered
  5. washThe filtercake is washed with isopropanol, THF, and acetone
  6. customrecrystallized from ethanol
  7. filtrationThe product is filtered off
  8. washwashed with ether
  9. customdried