HRID2236544

反应详情

EQUATION

反应方程式

HRID 2236544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-methoxy-4H-isoquinoline-1,3-dione (400 mg, 2.1 mmole), 8 mL of a 4:1 mixture of acetic anhydride and N,N-dimethylformamide and trimethylorthoformate (1.7 mL, 15.5 mmole) is stirred and heated to reflux. After 30 minutes the solvents are removed, the residue treated with hexane-ethyl acetate, the solid collected by filtration, washed with fresh hexane-ethyl acetate and dried to give a yellow solid, 317 mg, (65%), mp 245-7° C., MS (ESI): m/z 234.1 (M+H).

WORKUP

后处理

  1. temperatureheated to reflux
  2. customAfter 30 minutes the solvents are removed
  3. additionthe residue treated with hexane-ethyl acetate
  4. filtrationthe solid collected by filtration
  5. washwashed with fresh hexane-ethyl acetate
  6. customdried
  7. customto give a yellow solid, 317 mg, (65%), mp 245-7° C., MS (ESI)