HRID2118764

反应详情

EQUATION

反应方程式

HRID 2118764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.5 g of 5,8-dimethoxy-1,2,3,4-tetrahydro-2-hydroxy-2-naphthaleneacetic acid in 150 ml of tetrahydrofuran were added dropwise within 15 minutes to 3.32 g of lithium aluminum hydride in 150 ml of tetrahydrofuran. The reaction mixture was heated to reflux for 1 hour and then cooled. After the dropwise addition of 15 ml of ethyl acetate and 20 ml of water the suspension was filtered and the filtrate was concentrated. The product was purified by column chromatography (silica gel, chloroform/methanol 30:1). There was obtained 5,8-dimethoxy-1,2,3,4-tetrahydro-2-hydroxy-2-naphthaleneethanol, m.p. 121°-122°.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 1 hour
  3. temperaturecooled
  4. filtrationwas filtered
  5. concentrationthe filtrate was concentrated
  6. customThe product was purified by column chromatography (silica gel, chloroform/methanol 30:1)