反应详情

温度

50 °C

Trimethylsilylchloride (0.3 ml) is added at room temperature to a suspension of N-[4-methyl-5-(2-methyl-pyrimidin-4-yl)-thiazol-2-yl]-acetamide (29 mg, prepared as described in WO 04/096797) in ethanol (2 ml) at room temperature. The mixture is heated at 50° C. for 18 hours, conc. HCl (0.2 ml) is added and the heating at 50° C. is continued for a further 46 hours. Following cooing the mixture is partitioned between saturated aqueous NaHCO3 and CH2Cl2 containing 10% methanol and extracted a further 2×CH2Cl2. Evaporation of the organic layers gives the title compound as a beige solid. 1H nmr (d4-methanol, 400 MHz) 8.44 (d, J=7 hz, 1H), 7.33 (d, J=7 Hz, 1H), 2.58 (s, 3H), 2.51 (s, 3H).

1. customis partitioned between saturated aqueous NaHCO3 and CH2Cl2 containing 10% methanol
2. extractionextracted a further 2×CH2Cl2
3. customEvaporation of the organic layers