HRID2387911

反应详情

EQUATION

反应方程式

HRID 2387911 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of boron tribromide (13.95 ml, 1M in DCM) was added portionwise over 30 min to a stirred suspension of the product from example 83 step (iv) (1 g) in DCM (15 mL) at 0° C. The suspension was allowed to warm to rt and stirred for 5 h. The suspension was cooled to 0° C. and then MeOH (10 mL) and 4M HCl in dioxane (2 mL) were added and the mixture stirred for 1 h. The solvent was evaporated under reduced pressure and the residue was purified by flash silica chromatography (5% MeOH/DCM) to give the title compound (minor product) as a white solid, 51 mg.

WORKUP

后处理

  1. temperatureThe suspension was cooled to 0° C.
  2. stirringthe mixture stirred for 1 h
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by flash silica chromatography (5% MeOH/DCM)