反应详情

A mixture of 4-(2,4-dichlorophenyl)-2-morpholin-4-yl-1,3-thiazole-5-carboxamide (23 mg, 0.06 mmol) and 1,1-dimethoxy-N,N-dimethylmethanamine (0.8 mL, 6 mol) was irradiated in the microwave at 160° C. (300 watts) for 30 minutes. The reaction was concentrated in vacuo. The residue dissolved in acetic acid (1.0 mL, 0.18 mol) and hydrazine hydrate (30 mg, 0.7 mmol) and subjected to microwave irradiation at 120° C. (300 watts) for 15 minutes. The solvent was removed in vacuo, the residue was diluted with water (1 mL), the precipitate was collected, washed with water (1 mL) and dried to afford the title compound (10 mg, 40%). LCMS: (FA) ES+, 382. 1H NMR (400 MHz, d6-DMSO) δ: 13.9 (s, 1H), 8.42 (s, 1H), 7.63 (d, 1H), 7.44-7.42 (m, 2H), 3.73-3.70 (m, 4H), 3.44-3.42 (m, 4H).

1. customwas irradiated in the microwave at 160° C. (300 watts) for 30 minutes
2. concentrationThe reaction was concentrated in vacuo
3. customirradiation at 120° C. (300 watts) for 15 minutes
4. customThe solvent was removed in vacuo
5. additionthe residue was diluted with water (1 mL)
6. customthe precipitate was collected
7. washwashed with water (1 mL)
8. customdried