HRID345579

反应详情

EQUATION

反应方程式

HRID 345579 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 4.1 parts of ethyl 4-amino-5-cyano-2-hydroxybenzoate in 40 parts of 2-propanone were added successively 2.52 parts of dimethyl sulfate and 4.1 parts of potassium carbonate. The whole was stirred and refluxed for 3 hours. The reaction mixture was filtered while hot and the filter-cake was washed with 2-propanone. The filtrate was evaporated and the solid residue was crystallized from 24 parts of 2-propanol, yielding 3.5 parts (79.5%) of ethyl 4-amino-5-cyano-2-methoxybenzoate; mp. 164.5° C. (intermediate 110).

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. filtrationThe reaction mixture was filtered while hot and the filter-cake
  3. washwas washed with 2-propanone
  4. customThe filtrate was evaporated
  5. customthe solid residue was crystallized from 24 parts of 2-propanol