HRID1044505

反应详情

EQUATION

反应方程式

HRID 1044505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(1-(3,4-Dichlorobenzyl)-7-methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)pyrrolidine (1.6 g, 4.10 mmol) was dissolved in CH2Cl2 (100 ml) and BBr3 (1 molar in CH2Cl2, 12.3 ml, 12.3 mmol) was added at −10° C. It was stirred for 2 h after which time the temperature rose to room temperature. Ice water was added, the organic phase separated and the aqueous phase extracted with CH2Cl2. The combined organic layers were washed with saturated NaHCO3 and NaCl solution, dried over Na2SO4, and concentrated to afford a residue. The beige solid product (1.2 g, 78%) was obtained from precipitation in ethyl acetate.

WORKUP

后处理

  1. customrose to room temperature
  2. customthe organic phase separated
  3. extractionthe aqueous phase extracted with CH2Cl2
  4. washThe combined organic layers were washed with saturated NaHCO3 and NaCl solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customto afford a residue