HRID569082

反应详情

EQUATION

反应方程式

HRID 569082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Hydroxymethyl-4-methoxymethyl-beta-carboline-3-carboxylic acid ethyl ester (0.20 g) is dissolved in dichloromethane (5 ml). A solution of phosphorous tribromide (0.17 g) in dichloromethane (3 ml) is added drop by drop with stirring. After three hours of stirring, the mixture is cooled to +10° C. and mixed with a solution of morpholine (1.0 ml) in ethanol (5 ml) drop by drop. After standing overnight the solvent is evaporated, the residue is chromatographed on silica gel with a mixture of dichloromethane (19 parts) and ethanol (1 part) and the title compound (0.16 g) with a melting point of 195°-196° C. is obtained.

WORKUP

后处理

  1. stirringAfter three hours of stirring
  2. temperaturethe mixture is cooled to +10° C.
  3. customthe solvent is evaporated
  4. customthe residue is chromatographed on silica gel with a mixture of dichloromethane (19 parts) and ethanol (1 part)