HRID2074005

反应详情

EQUATION

反应方程式

HRID 2074005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A mixture of methyl 4-amino-5-chlorosalicylate (5 g), allyl bromide (12.6 g), ground K2CO3 (30 g) and acetone (120 ml) is stirred at reflux for 5 hours and cooled to 25° C. The mixture is partitioned between methylene chloride and H2O, the organic layer is separated, dried (MgSO4), filtered and evaporated. The residue is recrystallized from hexanechloroform affording the desired product as a crystalline solid (M.P. 107°-109° C.).

WORKUP

后处理

  1. temperatureat reflux for 5 hours
  2. customThe mixture is partitioned between methylene chloride and H2O
  3. customthe organic layer is separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is recrystallized from hexanechloroform