反应详情

A suspension of 4-chloro-N-[4-chloro-6-(4-chlorophenylamino)-pyrimidin-5-yl]-2-fluorobenzamide I-(7A-91)a (8.3 g, 20 mmol) in POCl3 (100 ml) was heated to reflux. The light brown reaction became homogeneous over 2 hours. After refluxing 3 hours, the reaction mixture was cooled and concentrated under reduced pressure to give a viscous oil. The residue was diluted with ethyl acetate and poured over ice/aqueous sodium bicarbonate. The organic layer was separated, washed with brine, dried (Na2SO4), and concentrated. Crystallization from diethyl ether afforded product I-(7A-91)b (5.8 g, 73%) as an off-white solid: +ESI MS (M+1) 393.0; 1H NMR (400 MHz, DMSO-d6) δ 8.81 (s, 1H), 7.72 (t, J=8.1 Hz, 1H), 7.60–7.55 (m, 3H), 7.50–7.42 (m, 3H).

1. customThe light brown reaction
2. temperatureAfter refluxing 3 hours
3. temperaturethe reaction mixture was cooled
4. concentrationconcentrated under reduced pressure
5. customto give a viscous oil
6. additionpoured over ice/aqueous sodium bicarbonate
7. customThe organic layer was separated
8. washwashed with brine
9. dry with materialdried (Na2SO4)
10. concentrationconcentrated
11. customCrystallization from diethyl ether afforded product I-(7A-91)b (5.8 g, 73%) as an off-white solid