反应详情

A round-bottom flask was charged with perfluorophenyl 1-(4-chloro-2-methoxyphenyl)isoquinoline-6-sulfonate (INTERMEDIATE NNN; 102.15 mg, 0.198 mmol), 1,3,4-thiadiazol-2-amine (40.1 mg, 0.396 mmol), cesium carbonate (194 mg, 0.594 mmol), and DMF (1 mL) (1:30 pm). The mixture was diluted with EtOAc and 0.5 N aq. HCl. The layers were separated, and the organic extract was washed with brine, dried over sodium sulfate, filtered, and concentrated. The residue was purified by chromatography on silica gel (12-g Redi-Sep Gold column, 0-7% MeOH/DCM) to give 1-(4-chloro-2-methoxyphenyl)-N-(1,3,4-thiadiazol-2-yl)isoquinoline-6-sulfonamide (64.78 mg, 0.150 mmol, 76% yield) as a white solid. m/z (ESI) 433.0 (M+H)+.

1. customThe layers were separated
2. extractionthe organic extract
3. washwas washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by chromatography on silica gel (12-g Redi-Sep Gold column, 0-7% MeOH/DCM)