HRID11079

反应详情

EQUATION

反应方程式

HRID 11079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bromination of 2-chloro-3-nitrotoluene with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 102, except that the reaction time for the bromination was 2 h and the displacement reaction was performed at 70° C. for 1 d, gave the phosphonium salt (554) (44%) as a light brown solid, mp (CH2Cl2/benzene) 224–228° C. 1H NMR (CDCl3) δ 8.09 (br d, J=8.3 Hz, 1H), 7.86–7.63 (m, 16H), 7.34 (t, J=8.1 Hz, 1H), 5.95 (d, J=14.6 Hz, 2H). Found: C, 58.68; H, 4.12; N, 2.79. C25H20BrclNO2P requires C, 58.56; H, 3.93; N, 2.73.

WORKUP

后处理

  1. customthe displacement reaction
  2. waitwas performed at 70° C. for 1 d