HRID1436561

反应详情

EQUATION

反应方程式

HRID 1436561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add a suspension of potassium peroxymonosulfate (35.6 g, 57.7 mmol) in water (80 mL) to a cooled solution of 2-chloro-6-propylsulfanyl-isonicotinic acid methyl ester (4.71 g, 19.2 mmol) in methanol (40 mL) and THF (40 mL). Stir the mixture at room temperature for 3 days. Dilute the mixture with water and extract with dichloromethane (3×100 mL). Wash the combined extracts with water, dry (magnesium sulfate), concentrate and purify (silica gel chromatograpy, eluting with 20:80 ethyl acetate:hexanes) to give the title product (2.75 g, 52%).

WORKUP

后处理

  1. additionAdd
  2. extractionextract with dichloromethane (3×100 mL)
  3. washWash the combined extracts with water
  4. dry with materialdry (magnesium sulfate)
  5. concentrationconcentrate
  6. custompurify
  7. wash(silica gel chromatograpy, eluting with 20:80 ethyl acetate:hexanes)