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

HRID 502087ノート

反応式

HRID 502087 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-[(triisopropylsilyl)-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 sulfate 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 sulfate the solvent
  3. customis removed
  4. customthe residue is purified

出典と根拠

ORDレコード
ord-fb657bb8a2d84b589804409eb0c78f31
出典データセット
uspto-grants-2010_08
特許番号
US07772378B2

反応ノート

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