反应详情

温度

0 °C

A suspension of 2,4-dichloro-N-[4-chloro-6-(4-chlorophenylamino)-pyrimidin-5-yl]-benzamide I-(1A-1)b (48 g, 0.11 mol) in acetic acid (1 l) was heated to reflux for 7 hours. The reaction mixture was cooled to 0° C., the product (colorless needles) was collected by vacuum filtration, and the solid was washed with additional acetic acid, ethyl acetate, and then ether. The product was dried overnight under high vacuum to afford the title compound I-(1A-1)c (32 g, 73%) as a colorless, fluffy solid. The mother liquor was concentrated under reduced pressure and the solid crystallized from methanol to provide additional material (16 g) as a colorless solid: mp 314–315° C.; +ESI MS (M+1) 391.3; 1H NMR: (400 MHz, CD3OD): δ 8.06 (s, 1H), 7.61 (d, J=8.3 Hz, 1H), 7.52 (d, J=2.1 Hz, 1H), 7.48–7.41 (m, 3H), 7.31 (d, J=8.7 Hz, 2H).

1. temperaturewas heated
2. temperatureto reflux for 7 hours
3. filtrationthe product (colorless needles) was collected by vacuum filtration
4. washthe solid was washed with additional acetic acid, ethyl acetate
5. customThe product was dried overnight under high vacuum