Trifluoroacetic acid → [4-(5-Bromo-2-fluoro-benzyl)-phenylethynyl]-triisopropyl-silane

HRID 2263589ノート

反応式

HRID 2263589 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:28])=[C:6]([CH:8]([C:10]2[CH:15]=[CH:14][C:13]([C:16]#[C:17][Si:18]([CH:25]([CH3:27])[CH3:26])([CH:22]([CH3:24])[CH3:23])[CH:19]([CH3:21])[CH3:20])=[CH:12][CH:11]=2)O)[CH:7]=1.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>ClCCl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:28])=[C:6]([CH:7]=1)[CH2:8][C:10]1[CH:15]=[CH:14][C:13]([C:16]#[C:17][Si:18]([CH:25]([CH3:27])[CH3:26])([CH:22]([CH3:23])[CH3:24])[CH:19]([CH3:20])[CH3:21])=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 57809581(5-Bromo-2-fluoro-phenyl)-{4-[(triisopropylsilyl)-ethynyl]-phenyl}methanol

生成物 1

HCID 16065645[4-(5-Bromo-2-fluoro-benzyl)-phenylethynyl]-triisopropyl-silane

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 5.6 g (5-bromo-2-fluoro-phenyl)-{4-[(triisopropylsily)-ethynyl]-phenyl}-methanol and 4.1 ml triethylsilane in 50 ml dichloromethane is cooled in an ice bath. Then 4.7 ml trifluoroacetic acid are slowly added dropwise, and the solution is stirred for 4 h at ambient temperature. The solution is diluted with dichloromethane and washed with aqueous sodium hydrogen carbonate solution. After drying over sodium sulphate the solvent is removed and the residue is purified using silica gel (cyclohexane).

後処理

  1. washwashed with aqueous sodium hydrogen carbonate solution
  2. dry with materialAfter drying over sodium sulphate the solvent
  3. customis removed
  4. customthe residue is purified

出典と根拠

ORDレコード
ord-02f273c064764e44ac1c49256f249a99
出典データセット
uspto-grants-2010_12
特許番号
US07851602B2

反応ノート

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