HRID1186207

反应详情

EQUATION

反应方程式

HRID 1186207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-fluoro-3-methyl-pyridine-2-carboxylic acid methyl ester (1.28 g) in MeOH (6 ml) was added at 22° C. a solution of lithium hydroxide mono hydrate (636 mg) in water (3 ml) and stiring was continued for 16 h. The mixture was diluted with water, the MeOH was evaporated at reduced pressure and the pH was adjusted to 1 using 1 N aqueous HCl. The aqueous layer was extracted with AcOEt, the organic layer was dried, evaporated and the residue was crystallized from AcOEt/n-heptane to give the title compound (1.02 g) as a pale yellow solid. MS: m/z=153.7 [M−H]−.

WORKUP

后处理

  1. customthe MeOH was evaporated at reduced pressure
  2. extractionThe aqueous layer was extracted with AcOEt
  3. customthe organic layer was dried
  4. customevaporated
  5. customthe residue was crystallized from AcOEt/n-heptane