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

HRID 1769565ノート

反応式

HRID 1769565 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 147662924-Octyl-2'-fluoro-4'-bromobiphenyl収率 71.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2782fb43374f41399aaaf810bc2ad426
出典データセット
uspto-grants-1995_01
特許番号
US05382380

反応ノート

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