Trifluoroacetic acid → 4-Octyl-2'-fluoro-4'-bromobiphenyl

HRID 1769565노트

반응식

HRID 1769565 반응식
[C:1]([C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19]([Br:22])=[CH:18][C:17]=2[F:23])=[CH:12][CH:11]=1)(=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].FC(F)(F)C(O)=O.C([SiH](CC)CC)C>O>[CH2:1]([C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][C:19]([Br:22])=[CH:18][C:17]=2[F:23])=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 189854264-Octanoyl-2'-fluoro-4'-bromobiphenyl

생성물 1

HCID 147662924-Octyl-2'-fluoro-4'-bromobiphenyl수율 71.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A reaction vessel was charged with 3.75 g of 4-octanoyl-2'-fluoro-4'-bromobiphenyl and 20 ml of trifluoroacetic acid. To the mixture was added dropwise 2.4 g of triethylsilane with stirring at room temperature. After stirring for 6 hours, the reaction liquid was poured into water and the mixture was extracted with benzene. The benzene extract was washed successively with water, an aqueous solution of sodium hydrogen carbonate and water, and then dried over Glauber's salt. The solvents were distilled off and the residue was distilled in a glass tube oven (GTO) to obtain 2.56 g (71.1%) of 4-octyl-2'-fluoro-4'-bromobiphenyl. GTO-set temperature: 150° C./0.2 mmHg.

후처리

  1. stirringAfter stirring for 6 hours
  2. customthe reaction liquid
  3. extractionthe mixture was extracted with benzene
  4. extractionThe benzene extract
  5. washwas washed successively with water
  6. dry with materialan aqueous solution of sodium hydrogen carbonate and water, and then dried over Glauber's salt
  7. distillationThe solvents were distilled off
  8. distillationthe residue was distilled in a glass tube oven (GTO)

출처 및 근거

ORD 기록
ord-2782fb43374f41399aaaf810bc2ad426
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05382380

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