反应详情

Sodium hydride (0.4 g of a 60% dispersion in oil) was added to a solution of 3-methoxy-2-pyrazinamine (0.25 g) in N-methylpyrrolidinone (10 mL). After 0.5 h, 2,3-dichloro-4-fluorobenzenesulphonyl chloride (Example 185a) (0.63 g) was added. After 16 h at room temperature the reaction mixture was quenched with 2M aqueous HCl, extracted with ethyl acetate, dried (MgSO4) and evaporated. Purification was by silica gel chromatography eluting with ethyl acetate/iso-hexane mixtures. Yield 0.16 g.

1. customAfter 16 h at room temperature the reaction mixture was quenched with 2M aqueous HCl
2. extractionextracted with ethyl acetate
3. dry with materialdried (MgSO4)
4. customevaporated
5. customPurification
6. washeluting with ethyl acetate/iso-hexane mixtures