反应详情

温度

150 °C

A mixture of 2-acetamido-5-chlorothiazole (14.3 g), 2-mercaptopyrimidine (10 g) and potassium carbonate anhydrous (22.4 g) in N,N-dimethylformamide (280 ml) was stirred at 150° C. an hour. The reaction mixture was poured into water with stirring under ice cooling. The mixture was extracted with ethyl acetate, washed with water and dried over magnesium sulfate. The organic layer was concentrated under reduced pressure to give solid. The solid was triturated with water, and the precipitates were collected by filtration, washed with water and dried in vacuo no give 2-acetamido-5-(2-pyrimidinylthio)thiazole (12.30 g, yield: 60.2%). mp: 225° C. (dec.) IR (Nujol): 3170, 1645, 1555, 1310 cm-1NMR (DMSO-d6, 60 MHZ, ppm): 2.20 (3H, s), 7.33 (1H, t, j=4 Hz), 7.70 (1H, s), 8.68 (2H, d, J=4 Hz), 12.33 (1H, br s) Mass: M+2 254, M+1 253, M 252, m/e 210, 168

1. stirringwith stirring under ice cooling
2. extractionThe mixture was extracted with ethyl acetate
3. washwashed with water
4. dry with materialdried over magnesium sulfate
5. concentrationThe organic layer was concentrated under reduced pressure
6. customto give solid
7. customThe solid was triturated with water
8. filtrationthe precipitates were collected by filtration
9. washwashed with water