HRID342868

反应详情

EQUATION

反应方程式

HRID 342868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from step (e) (20 g) was added to a 1M solution of lithium aluminium hydride (1.5 molar equivalents) in THF and the mixture reflexed for 3 hours, then stirred for 16 hours at room temperature. The mixture was cooled to about 0° C., then quenched with water and 1N aqu. NaOH added. The resulting solid was broken up with additional water and the suspension heated at 50° C. for 5 minutes, then cooled to room temperature, diethyl ether (100 ml) added and filtered. The filtrate was evaporated in vacuo to give the desired product as an oil (82% yield).

WORKUP

后处理

  1. temperatureThe mixture was cooled to about 0° C.
  2. customquenched with water and 1N aqu
  3. additionNaOH added
  4. temperaturethe suspension heated at 50° C. for 5 minutes
  5. temperaturecooled to room temperature
  6. additiondiethyl ether (100 ml) added
  7. filtrationfiltered
  8. customThe filtrate was evaporated in vacuo