HRID1598984

反应详情

EQUATION

反应方程式

HRID 1598984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 6-methoxy-1,3-benzodioxole-5-carboxylate (3 g, 14 mmol), prepared as in Example 1, 20% sodium hydroxide (50 mL) and ethanol (25 mL) was heated 1 hour at reflux and then diluted with water, washed with diethyl ether (2×), treated with concentrated hydrochloric acid and cooled in an ice-bath. The solids were collected, washed with water (2×) and dried under vacuum at 70° C. to give 6-methoxy-1,3-benzodioxole-5-carboxylic acid (2.3 g, 12 mmol), m.p. 151° C.

WORKUP

后处理

  1. temperaturewas heated 1 hour
  2. temperatureat reflux
  3. washwashed with diethyl ether (2×)
  4. additiontreated with concentrated hydrochloric acid
  5. temperaturecooled in an ice-bath
  6. customThe solids were collected
  7. washwashed with water (2×)
  8. customdried under vacuum at 70° C.