HRID274080

反应详情

EQUATION

反应方程式

HRID 274080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-one (220 g) in methanol (1300 ml) was added portionwise sodium borohydride (22.0 g) at 6° C.-30° C., and then the reaction mixture was stirred for 40 minutes and evaporated in vacuo. The residue was partitioned between ethyl acetate (1 l) and water (1 l). The organic layer was washed with 1N hydrochloric acid (500 ml), aqueous sodium hydrogen carbonate (500 ml), and brine (200 ml), and dried over magnesium sulfate. The solvent was evaporated in vacuo to give 3-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-ol as a white powder.

WORKUP

后处理

  1. customevaporated in vacuo
  2. customThe residue was partitioned between ethyl acetate (1 l) and water (1 l)
  3. washThe organic layer was washed with 1N hydrochloric acid (500 ml), aqueous sodium hydrogen carbonate (500 ml), and brine (200 ml)
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated in vacuo