Реакция #1605854

Уравнение реакции

hydrobromic acid

sulfuric acid

hydrobromic acid

[2′,6′-dimethyl-4′-[3-(methylsulfonyl)propoxy]-[1,1′-biphenyl]-3-yl]methanol

→

title compound

3′-(bromomethyl)-2,6-dimethyl-4-(3-(methylsulfonyl)propoxy)-1,1′-biphenyl

Растворители

water

Условия реакции

Обработка

1. 1
   workup.ADDITIONadded to the mixture
2. 2
   workup.STIRRINGThe mixture was further stirred for 1 hour at the same temperature
3. 3
   Температураto cool
4. 4
   ЭкстракцияThe mixture was extracted with ethyl acetate
5. 5
   ПромывкаThe obtained organic phase was washed with water
6. 6
   Промывкаwashed with brine
7. 7
   Сушкаdried over anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONFrom the organic phase, the solvent was distilled off under reduced pressure

Методика

Concentrated sulfuric acid (1.4 g) was added dropwise to 48% hydrobromic acid (15 ml) at room temperature and [2′,6′-dimethyl-4′-[3-(methylsulfonyl)propoxy]-[1,1′-biphenyl]-3-yl]methanol (25 g) synthesized in accordance with the method described in [WO 2008/001931 pamphlet] was divided into five portions and added to the mixture. The reaction mixture was stirred at 60° C. for 2.5 hours and 48% hydrobromic acid (3.3 ml) was added to the mixture. The mixture was further stirred for 1 hour at the same temperature. After the reaction mixture was allowed to cool, water was added to the reaction mixture. The mixture was extracted with ethyl acetate. The obtained organic phase was washed with water, then washed with brine, and dried over anhydrous sodium sulfate. From the organic phase, the solvent was distilled off under reduced pressure to give the title compound (27 g) as a pale yellow solid.

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