HRID58325

反应详情

EQUATION

反应方程式

HRID 58325 的结构方程式

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

(3-bromopropyl)(triphenyl)phosphonium bromide (4.9 g, 10.0 mmol) was treated with 7 M ammonia in methanol (97 mL, 680 mmol) in a sealed tube. The mixture was heated at 85° C. for 4 hours and cooled to room temperature. The volatiles were removed, and the resultant semi-solid was purified on a silica gel column eluting with first with 20% methanol in methylene chloride followed by 25% 1 M ammonia in methanol and methylene chloride to give the title compound (2.07 g) in a 41% yield.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. customThe volatiles were removed
  3. customthe resultant semi-solid was purified on a silica gel column
  4. washeluting with first with 20% methanol in methylene chloride