HRID1509300

反应详情

EQUATION

反应方程式

HRID 1509300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-bromo-7-phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one (0.26 g, 0.852 mmol) and Lawesson's Reagent (0.34 g, 0.852 mmol) in toluene (10 ml) was heated at 120 degree for 16 h. The reaction mixture was concentrated to dryness and was added DCM (5 ml) and diisopropyl ether (20 ml). The precipitate was filtered to give product (0.18 g). 1H NMR (500 MHz, DMSO-d6): 12.9 (br, 1H), 7.35-7.55 (m, 5H), 7.32 (s, 1H), 5.16 (s, 2H).

WORKUP

后处理

  1. temperaturewas heated at 120 degree for 16 h
  2. concentrationThe reaction mixture was concentrated to dryness
  3. additionwas added DCM (5 ml) and diisopropyl ether (20 ml)
  4. filtrationThe precipitate was filtered