HRID2300123

反应详情

EQUATION

反应方程式

HRID 2300123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Prepared by heating under reflux overnight a stirred mixture of 3-(4,4-dimethyl-2-oxo-1,2,3,4,-tetrahydroquinolin-6-yl)benzonitrile and an equal weight of phosphorus pentasulfide in pyridine and workup as in the previous example gave a yellow solid: mp 220-223° C. dec. 1H-NMR (DMSO-d6) δ 12.35 (s, 1H), 8.21 (s, 1H), 8.10 (d, 1H, J=6.0 Hz), 7.80 (d, 1H, J=7.9 Hz), 7.72 (s, 1H), 7.65 (m, 2H), 7.21 (d, 1H, J=8.4 Hz), 2.85 (s, 2H), 1.27 (s, 6H); MS (APCI (−)) m/z 291 [M−H]− Anal. Calc. For C18H16N2S 3H2O: C, 62.40, H, 6.40, N, 8.09. Found: C, 62.12, H, 4.88, N 7.77.

WORKUP

后处理

  1. customPrepared
  2. temperatureby heating
  3. temperatureunder reflux overnight