HRID2120750

反应详情

EQUATION

反应方程式

HRID 2120750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Prepared by coupling 3-fluorophenylboronic acid with an equivalent amount of 6-bromo-4,4-dimethyl-3,4-dihydo-1H-quinolin-2-one using a catalytic amount of tetrakis(triphenylphosphine)palladium (0) with overnight refluxing in toluene containing an equivalent amount of potassium carbonate dissolved in water. Work up in the usual manner followed by recrystallization from ethanol gave a gray solid: mp 190-192° C. 1H-NMR (DMSO-d6) δ 10.27 (s, 1H), 7.57 (s, 1H), 7.50 (r, 4H), 7.15 (m, 1H), 6.95 (d, 1H J=8.2 Hz), 2.39 (s, 2H), 1.29 (s, 6H); MS (APCI (−)) m/z 268 [M−H]− Anal. Calc. For C17H16FNO 0.25H2O: C, 74.57, H, 6.07, N, 5.12. Found: C, 74.86, H, 5.97, N 5.06.

WORKUP

后处理

  1. customPrepared
  2. customwith overnight
  3. customfollowed by recrystallization from ethanol
  4. customgave a gray solid