HRID1655066

反应详情

EQUATION

反应方程式

HRID 1655066 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

181.2 g of isopropylmercaptan are added dropwise at a temperature of 0° to +2° C. in the course of 25 minutes to a suspension of 324 g of anhydrous potassium carbonate and 335.6 g of 2,3-difluoropyridine in 4500 ml of dimethylformamide. After the reaction mixture has been stirred for 18 hours at room temperature, it is poured into a mixture of 8000 ml of ice-water and 4000 ml of ethyl acetate. The organic phase is subsequently separated off and washed with ice-water and then with ethyl acetate. The combined organic phases are dried with sodium sulfate and subsequently concentrated. Purification by column chromatography over silica gel with ethyl acetate/n-hexane (1:9) gives 362.9 g of 2-isopropylthio-3-fluoropyridine in the form of an oil.

WORKUP

后处理

  1. customThe organic phase is subsequently separated off
  2. washwashed with ice-water
  3. dry with materialThe combined organic phases are dried with sodium sulfate
  4. concentrationsubsequently concentrated
  5. customPurification by column chromatography over silica gel with ethyl acetate/n-hexane (1:9)