HRID1841

反应详情

EQUATION

反应方程式

HRID 1841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

670 mg of the compound obtained in EXAMPLE 9 are dissolved in 10 ml of methylene chloride, and 0.2 ml of triethylamine and 0.2 ml of propionyl chloride are then added, with stirring. After 15 minutes, the reaction mixture is washed with water and then with 10% Na2CO3 solution and the organic phase is dried over MgSO4 and concentrated under vacuum. The residue is chromatographed on silica gel H using DCM and then a DCM/MeOH mixture (97/3; v/v) as the eluent. The product obtained is taken up with DCM, acidified to pH 1 by the addition of hydrochloric ether and concentrated under vacuum to give 0.52 g of the expected hydrochloride after crystallization from pentane. M.p.=115° C. (dec.).

WORKUP

后处理

  1. washthe reaction mixture is washed with water
  2. dry with materialwith 10% Na2CO3 solution and the organic phase is dried over MgSO4
  3. concentrationconcentrated under vacuum
  4. customThe residue is chromatographed on silica gel H
  5. customThe product obtained
  6. concentrationconcentrated under vacuum