HRID638558

反应详情

EQUATION

反应方程式

HRID 638558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4.5 g of (5-bromomethylisoxazol-3-yl-4-fluorophenylmethanone in 100 ml of Et2O was added dropwise to a solution of 7 ml of morpholine in 300 ml of 50% acetone/Et2O. The resulting mixture was stirred at room temperature for 20 hours. This mixture was filtered and the volatiles evaporated to give a residue which was dissolved in 600 ml of Et2O. The organic solution was washed with water until it became neutral and then with saturated NaCl, and dried over Na2SO4 and concentrated in vacuo to give 4.3 g of a crystalline solid. A 3.6 g sample of the amine was recrystallized from 65 ml of 8% toluene/hexane to yield 2.4 g (64%) of crystals, m.p. 72°-74°.

WORKUP

后处理

  1. filtrationThis mixture was filtered
  2. customthe volatiles evaporated
  3. customto give a residue which
  4. washThe organic solution was washed with water until it
  5. dry with materialwith saturated NaCl, and dried over Na2SO4
  6. concentrationconcentrated in vacuo