反应 #304892

反应方程式

sodium hydrogencarbonate

phenyltrimethylammonium tribromide

1-[3-Methoxy-5-(pentafluorosulfanyl)phenyl]ethanone

water

→

title compound

收率 105.4%

2-Bromo-1-[3-methoxy-5-(pentafluorosulfanyl)phenyl]ethanone

收率 105.4%

溶剂

THF

反应条件

后处理

1. 1
   workup.STIRRINGAfter stirring at RT for 2 h
2. 2
   萃取extracted three times with EA
3. 3
   萃取The alkaline water phase was extracted 3× with EA
4. 4
   干燥The combined organic phases were dried over magnesium sulfate
5. 5
   过滤after the desiccant had been filtered off
6. 6
   其他dried under reduced pressure
7. 7
   其他The residue was purified by means of preparative HPLC (
8. 8
   萃取extracted three times with EA
9. 9
   干燥The combined organic phases were dried over magnesium sulfate
10. 10
    过滤after the desiccant had been filtered off
11. 11
    其他dried under reduced pressure

实验过程

1-[3-Methoxy-5-(pentafluorosulfanyl)phenyl]ethanone (O2.007; 1.63 g) was dissolved in THF (150 ml), and phenyltrimethylammonium tribromide (2.2 g) was added at RT while stirring. After stirring at RT for 2 h, the mixture was admixed with water, neutralized with sodium hydrogencarbonate solution and extracted three times with EA. The alkaline water phase was extracted 3× with EA. The combined organic phases were dried over magnesium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. The residue was purified by means of preparative HPLC (met. A). The product fractions, each of them clean, were combined, freed of the acetonitrile under reduced pressure, neutralized with sodium hydrogencarbonate and extracted three times with EA. The combined organic phases were dried over magnesium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 1.27 g of the title compound were isolated. LC-MS rt: 1.65 min [M+H]+: 354.9 (met. b)

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