反应详情

A mixture of N-(2-(benzo[d]isothiazol-3-ylamino)ethyl)-4-chloropicolinamide (50 mg) in morpholine (1 mL) was microwaved at 160° C. for 30 min. The reaction mixture was diluted with dichloromethane and washed with saturated sodium bicarbonate solution and water. The organic layer was dried over anhydrous sodium sulfate, filtered and the filtrate concentrated under reduced pressure. Purification by flash column chromatography, on silica gel, eluting with a mixture of 1% methanol in dichloromethane and selected fractions were combined and concentrated under reduced pressure to give N-(2-(benzo[d]isothiazol-3-ylamino)ethyl)-4-morpholinopicolinamide as a white solid. 1H NMR (300 MHz, DMSO-d6): 8.80 (broad s, 1H), 8.20 (m, 1H), 8.10 (m, 1H), 7.91 (m, 1H), 7.30-7.60 (m, 3H), 7.00 (m, 1H), 3.60-3.80 (m, 4H), 3.30 ppm (m, 8H). MW=383 confirmed by LC-MS, tr=8.06 min (Method Y) MH+=384.

1. customwas microwaved at 160° C. for 30 min
2. washwashed with saturated sodium bicarbonate solution and water
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under reduced pressure
6. customPurification by flash column chromatography
7. washon silica gel, eluting with a mixture of 1% methanol in dichloromethane
8. concentrationconcentrated under reduced pressure