HRID1462364

反应详情

EQUATION

反应方程式

HRID 1462364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 ml of concentrated ammonia solution are added to a solution of 1.7 g of crude α-[N-[2-(3-carbomethoxy-4-hydroxy-phenoxy)-1-methyl-ethyl]-aminomethyl]-benzyl alcohol in 10 ml of dioxan and the mixture is left to stand at room temperature for 60-70 hours. The reaction mixture is evaporated, the residue is dissolved in 75 ml of ethyl acetate and the solution is washed with 10 ml of saturated, aqueous sodium chloride solution. Evaporation of the organic phase yields crude α-[N-[2-(3-carbamoyl-4-hydroxy-phenoxy)-1-methyl-ethyl]aminomethyl]-benzyl alcohol as a mixture of diastereoisomers in the form of an oil and the latter is crystallised from a little ethyl acetate and is identical to the product obtained, for example, in Example 1; melting point 120°-140°.

WORKUP

后处理

  1. waitthe mixture is left
  2. customThe reaction mixture is evaporated
  3. dissolutionthe residue is dissolved in 75 ml of ethyl acetate
  4. washthe solution is washed with 10 ml of saturated, aqueous sodium chloride solution
  5. customEvaporation of the organic phase