HRID901101

反应详情

EQUATION

反应方程式

HRID 901101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a cold (0° C.) solution of 1-cyclopropylmethyl-piperidin-4-one (314 mg, 2 mmol, 1.0 eq.) in ethanol (4 mL) was added sodium borohydride (61 mg, 2 mmol, 0.75 eq.). The reaction mixture was stirred 16 h at room temperature. Water, sodium hydroxide and dichloromethane were added and the reaction mixture was stirred 2 h at room temperature. The aqueous layer was extracted with dichloromethane and the combined organic phases were dried over sodium sulfate, filtered then concentrated to dryness in vacuo to yield 160 mg (50%) of the tide compound as colorless oil, witch was used in the next step without further purification. MS (m/e): 156.3 (MH+, 100%).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred 2 h at room temperature
  2. extractionThe aqueous layer was extracted with dichloromethane
  3. dry with materialthe combined organic phases were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationthen concentrated to dryness in vacuo