反应详情

温度

0 °C

POCl3 (532 mL) was added drop-wise to DMF (1 L) at 0° C. over 1 h. The solution was stirred at 0° C. for 1 h, and then product (1-B) (200 g, 0.9 mol) was added in small portions while the reaction temperature was maintained below 5° C. After the addition, the reaction was heated to 80° C. and stirred for another 4 hours. The solution was poured into ice water, and the pH was adjusted to 7 with 2 M NaOH, while maintaining the temperature below 5° C. After standing overnight, the solid was filtered, washed with H2O, and dried in vacuo to give crude product (2-B) (46 g, 30%, for two steps) as a yellow solid. 1H NMR (300 MHz, d-DMSO): δ 14.14 (br, 1H), 10.27 (s, 1H), 8.52 (br, 1H), 4.38 (q, 2H), 1.35 (t, 3H). LC-MS (M+H)+=169.

1. temperaturewas maintained below 5° C
2. additionAfter the addition
3. temperaturethe reaction was heated to 80° C.
4. stirringstirred for another 4 hours
5. temperaturewhile maintaining the temperature below 5° C
6. waitAfter standing overnight
7. filtrationthe solid was filtered
8. washwashed with H2O
9. customdried in vacuo