HRID1369218

反应详情

EQUATION

反应方程式

HRID 1369218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To dry CH2Cl2 (30 mL) cooled in an ice bath was added diethylsulfide (0.38 mL, 3.3 mmol) followed by AlCl3 (438 mg, 3.3 mmol). To this solution was added dropwise a solution of ethyl (±)-10,11-dihydro-3-methoxy-2-methyl-5H-dibenzo[a,d]cycloheptene-10-acetate (200 mg, 0.6 mmole) in dry CH2Cl2 (6 mL), and the resulting mixture was stirred at RT for 2 hr. The reaction was quenched with 1.0 N HCl (10 mL), and the layers were separated. The organic layer was dried (MgSO4) and concentrated on the rotavap to give the title compound (100 mg, 56%) as a colorless oil: MS (ES) m/e 311.2 (M+H)+.

WORKUP

后处理

  1. customThe reaction was quenched with 1.0 N HCl (10 mL)
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated on the rotavap