HRID58325
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturecooled to room temperature
- customThe volatiles were removed
- customthe resultant semi-solid was purified on a silica gel column
- washeluting with first with 20% methanol in methylene chloride