反应 #168721

反应方程式

5-(3-Bromo-phenyl)-5-difluoromethyl-morpholin-3-one

P2S5

ethyl acetate

→

title compound

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

溶剂

pyridine

反应条件

后处理

1. 1
   温度The mixture was heated to 80° V for 2 hrs
2. 2
   其他Phases were separated
3. 3
   洗涤the organic phase was washed with 1 N HCl, saturated NaHCO3 solution and brine
4. 4
   干燥dried over Na2SO4
5. 5
   浓缩concentrated under reduced pressure

实验过程

5-(3-Bromo-phenyl)-5-difluoromethyl-morpholin-3-one (6.10 g, 19.93 mmol) was dissolved in 63 ml dry pyridine, and P2S5 (5.32 g, 23.91 mmol) was added. The mixture was heated to 80° V for 2 hrs. After completion, the mixture was put between ethyl acetate and 1 H HCl solution. Phases were separated and the organic phase was washed with 1 N HCl, saturated NaHCO3 solution and brine. The organic phases were combined, dried over Na2SO4 and concentrated under reduced pressure to yield the title compound as off-white solid. 1H-NMR (360 MHz, DMSO-d6): 8.60 (s, 1H, NH), 7.80-7.35 (m, 4H), 6.54 (t, 1H, CHF2), 4.45 (m, 2H), 4.28 (d, 1H), 4.12 (d, 1H); MS: 322 [(M+H)+].

来源