HRID337270

反应详情

EQUATION

反应方程式

HRID 337270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (3-(2,6-dimethylbenzyloxy)-2-methoxyphenyl)methanol (Step B, 9.5 g, 32.7 mmol) and triethylamine (5.80 g, 57.4 mmol) in dry CH2Cl2 (100 ml) was added drop wise methanesulfonyl chloride (3.5 ml, 45 mmol) at 0° C. under argon. The reaction mixture was warmed to room temperature for 6 hours or until all the starting material is consumed, neutralized with cooled 10% Na2CO3 and extracted with CH2Cl2. The organic layer was concentrated, and purified by flash chromatography on a silica gel column (hex: methylene chloride 2:1) to give the title compound as light yellow oil

WORKUP

后处理

  1. customis consumed
  2. temperaturewith cooled 10% Na2CO3
  3. extractionextracted with CH2Cl2
  4. concentrationThe organic layer was concentrated
  5. custompurified by flash chromatography on a silica gel column (hex: methylene chloride 2:1)