HRID2113758

反应详情

EQUATION

反应方程式

HRID 2113758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

4-(Trifluoromethoxy)aniline (0.94 mmol, 177 mg) dissolved in dry CH3CN (2 mL) was added to crude 3-chloro-4-phenyl-1-(pyridin-3-ylmethyl)-1H-pyrrole-2,5-dione (0.47 mmol, 140 mg) and the reaction mixture was sequentially subjected to microwave heating single node 140° C. for 20 min, 140° C. for 120 min, and 140° C. for 120 min. 0.3 mL Water was added and the reaction mixture was purified using HPLC (57% 0.1M ammonium acetate buffer: 43% CH3CN→100% CH3CN, 20 mL/min) to give 92 mg (45%) of the title compound. 1H NMR (400 MHz, CD3CN) δ 8.63 (d, 1H), 8.52 (dd, 1H), 7.95 (bs, 1H), 7.80-7.74 (m, 1H), 7.37-7.32 (m, 1H), 7.19-7.08 (m, 3H), 7.01-6.95 (m, 2H), 6.94-6.88 (m, 2H), 6.84-7.78 (m, 2H), 4.77 (s, 2H).

WORKUP

后处理

  1. customthe reaction mixture was purified