HRID496435

反应详情

EQUATION

反应方程式

HRID 496435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(chloromethyl)-6-hydroxy-3,4-dihydro-1(2H)-naphthalenone (10.0 g, 48 mmol), sodium phenylsulfinate (23.4 g, 142 mmol) and acetonitrile (100 mL) was stirred at reflux under nitrogen overnight. The mixture was poured onto ice. The precipitate was isolated by filtration, air dried, and crystallized from methanol-dichloromethane-ethyl acetate to give 6-hydroxy-5-[(phenylsulfonyl)methyl]-3,4-dihydro-1(2H)-naphthalenone as a cream solid, 12.16 g, 84% yield. NMR spectrum was consistent with structure.

WORKUP

后处理

  1. temperatureat reflux under nitrogen overnight
  2. additionThe mixture was poured onto ice
  3. customThe precipitate was isolated by filtration, air
  4. customdried
  5. customcrystallized from methanol-dichloromethane-ethyl acetate