HRID274082

反应详情

EQUATION

反应方程式

HRID 274082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (R)-3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl acetate (136 g) in methanol (1.36 l) was added dropwise a solution of sodium hydroxide (46.4 g) in water (232 ml) at ambient temperature. The reaction mixture was stirred for 1 hour and evaporated in vacuo. The residue was partitioned between ethyl acetate (1.1 l) and brine (550 ml). The organic layer was washed with 1N hydrochloric acid solution (550 ml), 1N aqueous sodium hydroxide solution (550 ml), and brine (550 ml), dried over magnesium sulfate, and evaporated in vacuo to give (R)-3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ol (108.96 g) as a white powder.

WORKUP

后处理

  1. customevaporated in vacuo
  2. customThe residue was partitioned between ethyl acetate (1.1 l) and brine (550 ml)
  3. washThe organic layer was washed with 1N hydrochloric acid solution (550 ml), 1N aqueous sodium hydroxide solution (550 ml), and brine (550 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo