HRID429819

反应详情

EQUATION

反应方程式

HRID 429819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
7.5 °C

PROCEDURE

实验过程

A solution of 1.0 M lithium aluminum hydride (200 ml, 0.2 mole) in tetrahydrofuran was added dropwise to a solution of 1-methanesulfonylpiperidine-4-carboxylic acid ethyl ester (68 grams, 0.29 mole) in tetrahydrofuran (500 ml) at about +5° C. The reaction mixture was stirred at 5-10° C. for 15 minutes. Water (10 ml) was added dropwise and the mixture was filtered. The filtrate was concentrated under reduced pressure and triturated with 50% ethyl ether-hexane (100 ml). The resulting white solid was collected and dried to give 1-methanesulfonylpiperidine-4-methanol (46 grams, 82%), m.p. 96-97° C.

WORKUP

后处理

  1. filtrationthe mixture was filtered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customtriturated with 50% ethyl ether-hexane (100 ml)
  4. customThe resulting white solid was collected
  5. customdried