HRID737103

反应详情

EQUATION

反应方程式

HRID 737103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

The above compound could be made in the following manner: 1 eq. 2-Benzyl-morpholine-4-carboxylic acid tert-butyl ester could be dissolved in 4N solution of hydrogen chloride in dioxane and the mixture could be stirred at 60° C. for 3 h. The solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution could be added to the resulting residue, and the mixture could be washed with diethyl ether. The aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution and extracted with methylene chloride. The organic layer could be washed with brine and dried over sodium sulfate. After filtering, the material could be purified by column chromatography.

WORKUP

后处理

  1. customThe solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution
  2. additioncould be added to the resulting residue
  3. washthe mixture could be washed with diethyl ether
  4. additionThe aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution
  5. extractionextracted with methylene chloride
  6. washThe organic layer could be washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationAfter filtering
  9. customthe material could be purified by column chromatography