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

HRID 326962ノート

反応式

HRID 326962 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

In a reactor were placed 3.75 g of 4-octanoyl-2'-fluoro-4'-bromobiphenyl and 20 ml of trifluroacetic acid, to which was added 2.4 g of triethylsilane at room temperature and stirred for 6 hours. Then, the reaction solution was added into water, extracted into benzene, washed sequentially with water, aqueous sodium hydrogencarbonate, and again water, and dehydrated over Glauber's salt. After the solvent was distilled off, the residue was evaporated in a glass tube oven (GTO) to obtain 2.56 g of 4-octyl-2'-fluoro-4'-bromobiphenyl (71.1%).

後処理

  1. customIn a reactor were placed
  2. extractionextracted into benzene
  3. washwashed sequentially with water, aqueous sodium hydrogencarbonate, and again water
  4. distillationAfter the solvent was distilled off
  5. customthe residue was evaporated in a glass tube oven (GTO)

出典と根拠

ORDレコード
ord-2217cc47ec4d4b8f847a904bcca84492
出典データセット
uspto-grants-1993_12
特許番号
US05271867

反応ノート

読み込み中…