HRID1594522

反应详情

EQUATION

反应方程式

HRID 1594522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To the title compound of Example 19 Step C (0.11 mmol, 50 mg) in CH2Cl2 (0.5 mL) cooled to −78° C. was added dropwise BBr3 (0.33 mol, 330 μL of a 1 M solution in CH2Cl2). After addition, the reaction was removed from the cold bath for 30 min, then cooled to −78° C. and diluted with MeOH. The mixture was concentrated under reduced pressure and the product was isolated by chromatography on silica eluting with 4% MeOH in CH2Cl2 as a white solid. LC-MS (ESI, Method B): 1.80 min, m/z 456.1 (M+1).

WORKUP

后处理

  1. additionAfter addition
  2. customthe reaction was removed from the cold bath for 30 min
  3. additiondiluted with MeOH
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customthe product was isolated by chromatography on silica eluting with 4% MeOH in CH2Cl2 as a white solid
  6. custom1.80 min, m/z 456.1 (M+1)