HRID1973675

反应详情

EQUATION

反应方程式

HRID 1973675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.49 g of potassium are dissolved with heating in 60 cc of tert.butanol. After cooling, 1.5 g of 1-tert.butylamino-2,3-dihydroxypropane was added and subsequently 1.85 g of 4-chloro-2-methylthieno[3,2-c]pyridine was added. After stirring for one day at room temperature, heating is effected to 50° for a further day. The reaction solution is concentrated in a vacuum, the residue is taken up in 1 N hydrochloric acid and ether, the aqueous phase is neutralized with 2 N soda solution and extracted with methylene chloride. After drying over magnesium sulphate and concentrating, the title compound is obtained as an oil, which yields the hydrogen maleate having an M.P. of 210°-213°, with maleic acid in tetrahydrofuran.

WORKUP

后处理

  1. temperatureAfter cooling
  2. temperatureheating
  3. waitis effected to 50° for a further day
  4. concentrationThe reaction solution is concentrated in a vacuum
  5. extractionextracted with methylene chloride
  6. dry with materialAfter drying over magnesium sulphate
  7. concentrationconcentrating