HRID1285120

反应详情

EQUATION

反应方程式

HRID 1285120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 30 mg 4-chloro-2-methylthiopyrazolo(1,5-a)-1,3,5-triazine and 33 mg free histamine in 3 ml of methanol is stirred at room temperature overnight. After evaporation of solvent, the residue is dissolved in ethylacetate, washed with water, and dried over MgSO4. After removal of solvent, the residue is subject to silica gel preparative thin layer chromatography using CHCl3 /methanol=9:1 as a developing solvent. Appropriate fractions are isolated, extracted with CHCl3 /CH3OH (3:1), and solvent removed in vacuo to dryness. 20 mg of a white solid are recovered. TLC (silica gel CHCl3 /CH3OH=3:1) Rf=0.15.

WORKUP

后处理

  1. customAfter evaporation of solvent
  2. dissolutionthe residue is dissolved in ethylacetate
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. customAfter removal of solvent
  6. customAppropriate fractions are isolated
  7. extractionextracted with CHCl3 /CH3OH (3:1), and solvent
  8. customremoved in vacuo to dryness
  9. custom20 mg of a white solid are recovered