1-Ethynyl-4-fluorobenzene → HCID 19914695, 화합물

HRID 1090115노트

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HRID 1090115 반응식
[CH:1]([N:4]=[N+:5]=[N-:6])([CH3:3])[CH3:2].[F:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]#[CH:15])=[CH:10][CH:9]=1>>[F:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:6]=[N:5][N:4]([CH:1]([CH3:3])[CH3:2])[CH:15]=2)=[CH:10][CH:9]=1

참가 물질

3

실험 절차

A mixture of isopropylazide [G. A. Olah, D. J. Donovan, J. Org. Chem., 43, 860, (1978)] (54.5 g; 640.3 mmol) and 4-fluorophenylacetylene [J. B. Lambert et al., J. Am. Chem. Soc., 107, 5443, (1985)] (39 g; 325.1 mmol) was heated at 70° C. for 41 hours. The excess of isopropylazide was distilled off an the resultant crude compound was purified by chromatography on silica gel (230-400 mesh), eluent methylene chloride:acetone=39:1, giving the title compound (m.p. 54°-55° C.).

후처리

  1. distillationThe excess of isopropylazide was distilled off an the resultant crude compound
  2. customwas purified by chromatography on silica gel (230-400 mesh), eluent methylene chloride

출처 및 근거

ORD 기록
ord-26f3411848e34974b334fd095e1ab1be
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05081136

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