HRID2170520

反应详情

EQUATION

反应方程式

HRID 2170520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1-(1-benzyl-7-methoxy-3,4-dihydro-1H-naphthalen-2-ylidene)-pyrrolidinium bromide and AcOH (300 mL) in DCM (500 mL), H2O (3000 mL) and MeOH (500 mL) was stirred at reflux for 10 hrs. The aqueous layer was washed with DCM (1000 mL), and the combined organic layers were washed with water, dried over Na2SO4 and concentrated to give crude product, purified by silica gel chromatography to give 1-benzyl-7-methoxy-3,4-dihydro-1H-naphthalen-2-one (195 g, yield 53%) as yellow solid.

WORKUP

后处理

  1. temperatureat reflux for 10 hrs
  2. washThe aqueous layer was washed with DCM (1000 mL)
  3. washthe combined organic layers were washed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customto give crude product
  7. custompurified by silica gel chromatography