HRID458246

反应详情

EQUATION

反应方程式

HRID 458246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Chloromethyl-2-methoxy-1-pent-2-ynyloxy-benzene (28 g, 0.12 mol) and N-hydroxyphthalimide (19.5 g, 0.12 mol) are dissolved in 180 ml of N,N-dimethylformamide. The reaction mixture is heated to +70° C. and potassium hydroxide (24 ml of a 5 M solution in methanol, 0.12 mol) is added at this temperature. The reaction is stirred for 1 hour at +70° C., subsequently cooled to room temperature and poured on water. This mixture is stirred for one further hour and filtered. The resulting crystalls are washed with water and recrystallized from methanol/acetone (8:1) to yield 2-(3-methoxy-4-pent-2-ynyloxy-benzyloxy)-isoindole-1,3-dione as colourless crystalls.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated to +70° C.
  2. additionpoured on water
  3. stirringThis mixture is stirred for one further hour
  4. filtrationfiltered
  5. washThe resulting crystalls are washed with water
  6. customrecrystallized from methanol/acetone (8:1)