HRID868206

反应详情

EQUATION

反应方程式

HRID 868206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine the product of step A (12.2 g) with sodium azide (3.9 g) in DMF (200 ml). Stirr 44 hours, extract with ethyl acetate, wash with water, dry the organic layer over MgSO4 and concentrate. Dissolve the resultant residue in ethanol (150 ml), add 5.0 g 10% Pd/C and hydrogenate at 3 atm for 4 hours. Filter and concentrate the filtrate to obtain 2-(2-aminoethyl)-6-chloro-3,4-dihydro-1,1-dioxo-7-sulfamoyl-1,2,4-benzothiadiazine.

WORKUP

后处理

  1. extractionStirr 44 hours, extract with ethyl acetate
  2. washwash with water
  3. dry with materialdry the organic layer over MgSO4
  4. concentrationconcentrate
  5. dissolutionDissolve the resultant residue in ethanol (150 ml)
  6. additionadd 5.0 g 10% Pd/C
  7. filtrationFilter
  8. concentrationconcentrate the filtrate