HRID1044405

反应详情

EQUATION

反应方程式

HRID 1044405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-chloropyridin-2(1H)-one (100 mg, 0.77 mmol), K2CO3 (320 mg, 2.32 mmol) and (4-chlorophenyl)methanethiol (612 mg, 3.86 mmol) was stirred at 100° C. for 18 hours. After cooling the reaction to RT and was dilution with CH2Cl2 (5 mL), the crude product was subjected to flash chromatography (silica gel/hexane-EtOAc 100:0 to 0:100 gradient, employing LC-MS to identify the fractions containing the desired product) to afford 4-(4-chlorobenzylthio)pyridin-2(1H)-one 8A (96 mg, 46.9% yield). 1H NMR (400 MHz, Chloroform-D) δ ppm 12.30 (1H, br. s.), 7.28-7.43 (4H, m), 7.15 (1H, d, J=7.03 Hz), 6.28 (1H, d, J=1.51 Hz), 6.11 (1H, dd, J=6.90, 1.88 Hz), 4.11 (2H, s).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe reaction to RT