HRID745494

反应详情

EQUATION

反应方程式

HRID 745494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6.04 g of 3-(2-amino-2-methylpropoxy)-6-chloropyridazine obtained in Example 1, (a) and 5.95 g of 1-(2-chloro-3-methylphenoxy)-2,3-epoxypropane in 120 ml of methanol was refluxed for 3 hours. The solvent was evaporated under reduced pressure. A solution of the residue in benzene was extracted with 175 ml of 0.2N hydrochloric acid. The aqueous layer was made alkaline with potassium carbonate and extracted with chloroform. The chloroform layer was dried over sodium sulfate. The solvent was evaporated and the residue (10 g) was purified by column chromatography (50 g of Florisil; eluted with chloroform) to give 7.98 g of 1-(2-chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol as a colorless oil.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. extractionA solution of the residue in benzene was extracted with 175 ml of 0.2N hydrochloric acid
  3. extractionextracted with chloroform
  4. dry with materialThe chloroform layer was dried over sodium sulfate
  5. customThe solvent was evaporated
  6. customthe residue (10 g) was purified by column chromatography (50 g of Florisil; eluted with chloroform)