反应 #168709

反应方程式

5-(3-bromo-phenyl)-5-fluoromethyl-morpholin-3-one

Lawesson's reagent

→

title compound

5-(3-Bromo-phenyl)-5-fluoromethyl-morpholine-3-thione

溶剂

THF

反应条件

后处理

1. 1
   其他evaporated
2. 2
   其他The residue was chromatographed on silica gel (cyclohexane/EtOAc=15:1)

实验过程

A mixture of 5-(3-bromo-phenyl)-5-fluoromethyl-morpholin-3-one (1.52 g, 5.28 mmol) and Lawesson's reagent (2.14 g, 5.28 mmol) in 21 ml of THF was heated at 50° C. for 1 h and then evaporated. The residue was chromatographed on silica gel (cyclohexane/EtOAc=15:1) to give the title compound in the form of a colourless foam. TLC (hexane/EtOAc=3:1): Rf=0.21; HPLC: RtH2=3.49 min; 1H-NMR (400 MHz, CD3OD): 7.65 (s, 1H), 7.58 (d, 1H), 7.47 (d, 1H), 7.39 (t, 1H), 4.87 (s, 2H), 4.63 (d, 1H), 4.50 (s, 2H), 4.02 (d, 1H); MS: 304, 306 [(M+H)+].

来源