HRID707011
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
To a solution of EXAMPLE 329C (706 mg) in N,N-dimethylformamide (6 mL) was added NaH (60% in mineral oil, 300 mg). The mixture was stirred for 30 minutes, and then 5,6-dichloropyridine-3-sulfonamide (706 mg) was added. The mixture was stirred overnight. The mixture was poured over aqueous NH4Cl and extracted with ethyl acetate (3×200 mL). The combined organic layers were washed with water, brine and dried over Na2SO4. After filtration and evaporation of the solvent the residue was loaded on a silica gel cartridge and eluted with 5 to 10% 7N NH3 in methanol in dichloromethane to provide the title compound.
WORKUP
后处理
- stirringThe mixture was stirred overnight
- extractionextracted with ethyl acetate (3×200 mL)
- washThe combined organic layers were washed with water, brine
- dry with materialdried over Na2SO4
- filtrationAfter filtration and evaporation of the solvent the residue
- washeluted with 5 to 10% 7N NH3 in methanol in dichloromethane