HRID656753

反应详情

EQUATION

反应方程式

HRID 656753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To (3-benzyloxy-5-chloro-phenyl)-acetic acid methyl ester (8 g, 28 mmol) in CH2Cl2 (100 mL) at 0° C. was added boron tribromide (1M in CH2Cl2; 56 mL, 56 mmol). The reaction mixture was warmed to room temperature over 30 minutes and stirred for 2 hours. Once no starting material was seen by analytical LCMS and tlc, the mixture was cooled to 0° C. and quenched with H2O (50 mL). The volume was reduced, and the residue was diluted with EtOAc (500 mL). The solid material was filtered, and the organic layer was separated and concentrated. The crude material was purified by silica gel chromatography to give the title compound.

WORKUP

后处理

  1. temperaturethe mixture was cooled to 0° C.
  2. customquenched with H2O (50 mL)
  3. additionthe residue was diluted with EtOAc (500 mL)
  4. filtrationThe solid material was filtered
  5. customthe organic layer was separated
  6. concentrationconcentrated
  7. customThe crude material was purified by silica gel chromatography