HRID1733811

反应详情

EQUATION

反应方程式

HRID 1733811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl 3-trifluoromethylbenzylphosphonate (3.0 g, 10.0 mmol) was dissolved in a mixture; of 50 mL of conc hydrochloric acid and 1.5 mL of EtOH and was heated at reflux for 17 hours. After cooling the clear reaction mixture in an ice-water mixture, the white crystalline solid which formed was collected to give 2.05 g (84.3%) of the analytical product, mp=163°-164° C. 300 MHz 1H NMR (DMSO-D6) δ, 7.40-7.75 (m, 4H, aromatic), 3.09 (d, 2H, J=21.5 Hz, PCH2). D.C.I.M.S.[MH+, 241].

WORKUP

后处理

  1. temperatureat reflux for 17 hours
  2. customthe white crystalline solid which formed
  3. customwas collected