HRID2042416

反应详情

EQUATION

反应方程式

HRID 2042416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

trans-4-[2-(4-Furo[3,2-c]pyridin-4-yl-piperazin-1-yl)-ethyl]-cyclohexylamine trihydrochloride (intermediate A) (150 mg, 0.34 mmol) was dissolved in CH2Cl2 (1.5 ml) and the solution was cooled to 0° C. Et3N (139 mg, 1.37 mmol) and methanesulfonyl chloride (78 mg, 0.68 mmol) were added and the reaction mixture was stirred over night at room temperature. H2O was added and the product was extracted with CH2Cl2. The organic layer was dried (Na2SO4) and the solvent was evaporated. Purification by flash chromatography over silica gel (CH2Cl2/MeOH/25% NH3 aq 140:10:1) yielded the title compound as a white solid (78 mg, 56%), MS (ISP) m/z=407.2 [(M+H)+].

WORKUP

后处理

  1. extractionthe product was extracted with CH2Cl2
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. customthe solvent was evaporated
  4. customPurification by flash chromatography over silica gel (CH2Cl2/MeOH/25% NH3 aq 140:10:1)