HRID1651255

反应详情

EQUATION

反应方程式

HRID 1651255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of crude 7-methoxy-1-(3-methoxyphenyl)-2-naphthalenecarboxylic acid ethyl ester (4.1 g) in a mixture of methanol (20 mL) and 4N potassium hydroxide (5 mL) was heated at reflux for 3 hours. After the methanol was evaporated off, the reaction was diluted with water and extracted with ether (2×25 mL). The aqueous layer was acidified, extracted with dichloromethane (3×25 mL) and the dried (MgSO4) extracts evaporated to give 3.9 g of crude 7-methoxy-1-(3-methoxyphenyl)-2-naphthalenecarboxylic acid. Crystallization from toluene-hexane provided 3.05 g of acid, mp 164°-168° C. Anal. Calcd for C19H16O4 : C, 74.01; H, 5.23 Found: C, 73.58; H, 5.49

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customAfter the methanol was evaporated off
  4. additionthe reaction was diluted with water
  5. extractionextracted with ether (2×25 mL)
  6. extractionextracted with dichloromethane (3×25 mL)
  7. dry with materialthe dried (MgSO4)
  8. customextracts evaporated