HRID978650

反应详情

EQUATION

反应方程式

HRID 978650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 13.3 gm 5-bromophthalide and 12.7 gm N-bromosuccinimide in 480 ml carbon tetrachloride was irradiated with a tungsten floor lamp and refluxed for 3 hours. The reaction was followed by NMR. The succinimide was filtered off and the cake washed with carbon tetrachloride. The solvent was removed in vacuo leaving a residue of 19.2 gm, to which was added 100 ml water. This mixture was refluxed with stirring for 4 hours, then the mixture was cooled and the product filtered off, washed neutral with water and dried. Wt=9.9 gm.

WORKUP

后处理

  1. customwas irradiated with a tungsten floor lamp
  2. temperaturerefluxed for 3 hours
  3. filtrationThe succinimide was filtered off
  4. washthe cake washed with carbon tetrachloride
  5. customThe solvent was removed in vacuo
  6. customleaving a residue of 19.2 gm
  7. temperatureThis mixture was refluxed
  8. temperaturethe mixture was cooled
  9. filtrationthe product filtered off
  10. washwashed neutral with water
  11. customdried