HRID868206
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionStirr 44 hours, extract with ethyl acetate
- washwash with water
- dry with materialdry the organic layer over MgSO4
- concentrationconcentrate
- dissolutionDissolve the resultant residue in ethanol (150 ml)
- additionadd 5.0 g 10% Pd/C
- filtrationFilter
- concentrationconcentrate the filtrate