Tetrabutylammonium Fluoride → 1,3,5-Trichloro-2-ethynylbenzene

HRID 735086ノート

反応式

HRID 735086 の反応式
C1([Si](C2C=CC=CC=2)(C2C=CC=CC=2)[C:8]#[C:9][C:10]2[C:15]([Cl:16])=[CH:14][C:13]([Cl:17])=[CH:12][C:11]=2[Cl:18])C=CC=CC=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1>[Cl:16][C:15]1[CH:14]=[C:13]([Cl:17])[CH:12]=[C:11]([Cl:18])[C:10]=1[C:9]#[CH:8]

参加物

4

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 86060684Triphenyl-(2,4,6-trichlorophenylethynyl)silane

生成物 1

HCID 193780291,3,5-Trichloro-2-ethynylbenzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A reaction mixture of 5 g (10.8 mmol) of triphenyl-(2,4,6-trichlorophenylethynyl)silane and 4.2 g (16.2 mmol) of tetrabutylammonium fluoride in 50 mL of absolute THF is stirred for half an hour at ambient temperature and then evaporated down. The residue is taken up in diethyl ether and water and extracted. The organic phase is dried over sodium sulfate. The purification is carried out by column chromatography on silica gel (eluant: petroleum ether/toluene (9:1)). Yield: 0.46 g (20.7% of theory); Rf value: 0.6 (silica gel, petroleum ether/toluene (9:1)).

後処理

  1. customevaporated down
  2. extractionwater and extracted
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customThe purification

出典と根拠

ORDレコード
ord-427c66677cd246d5bb7cf7e5312da80a
出典データセット
uspto-grants-2009_09
特許番号
US07592373B2

反応ノート

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