HRID627732

反应详情

EQUATION

反应方程式

HRID 627732 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 methyl 5-(difluoromethoxy)picolinate (0.750 g, 3.69 mmol) in 1,4-dioxane (18.46 ml) was added sodium hydroxide, 1N aqueous solution (7.4 ml, 7.4 mmol) and the reaction mixture was stirred at RT for overnight. Then hydrogen chloride, 4.0M solution in 1,4-dioxane (1.8 ml, 7.38 mmol) was added and stirred for 1 h. The reaction mixture was concentrated and was diluted with water and extracted with EtOAc. The organic extract was dried over MgSO4, filtered and concentrated to give 5-(difluoromethoxy)picolinic acid (0.6013 g, 3.18 mmol, 86% yield). MS m/z: 190.2 [M+H].

WORKUP

后处理

  1. stirringstirred for 1 h
  2. concentrationThe reaction mixture was concentrated
  3. additionwas diluted with water
  4. extractionextracted with EtOAc
  5. extractionThe organic extract
  6. dry with materialwas dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated