HRID2222112

反应详情

EQUATION

反应方程式

HRID 2222112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-chloro-2-methoxybenzoic acid (1 mmol), oxalyl chloride (1 mmol), and DMF (0.05 mmol) in 2 mL of CH2Cl2 was stirred at rt for 6 h and then evaporated. To the residue was added 2 mL of CH2Cl2, triethylamine (2 mmol) and diethyl (hydroxymethyl)phosphonate (0.33 mmol) and this mixture was stirred at rt for 16 h and then diluted with water and CH2Cl2. The organic layer was dried (MgSO4) and evaporated. Purification of the residue by silica gel chromatography provided diethylphosphonomethyl 4-chloro-2-methoxybenzoate as an oil.

WORKUP

后处理

  1. customevaporated
  2. stirringthis mixture was stirred at rt for 16 h
  3. dry with materialThe organic layer was dried (MgSO4)
  4. customevaporated
  5. customPurification of the residue by silica gel chromatography