HRID745495

反应详情

EQUATION

反应方程式

HRID 745495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.6 g of 3-(2-amino-2-methylpropoxy)-6-chloropyridazine obtained in Example 1 (a) and 5.0 g of 1-(2-chloro-5-methylphenoxy)-2,3-epoxypropane in 50 ml of ethanol was refluxed for 4 hours. The solvent was evaporated under reduced pressure a solution of the residue in 100 ml of benzene was extracted with 30 ml of 10% hydrochloric acid. The aqueous layer was made alkaline with 10% sodium hydroxide and extracted with chloroform, and the organic layer was dried over magnesium sulfate. The solvent was evaporated and the residue was chromatographed on a column of Florisil (50 g) using chloroform as an eluent. From the eluate was obtained 5.7 g of 1-(2-chloro-5-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 a solution of the residue in 100 ml of benzene
  2. extractionwas extracted with 30 ml of 10% hydrochloric acid
  3. extractionextracted with chloroform
  4. dry with materialthe organic layer was dried over magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe residue was chromatographed on a column of Florisil (50 g)