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

HRID 735086노트

반응식

HRID 735086 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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)).

후처리

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

출처 및 근거

ORD 기록
ord-427c66677cd246d5bb7cf7e5312da80a
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07592373B2

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