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Water → HCID 19858048, 화합물

HRID 2073399
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HRID 2073399 반응식
[CH3:1][C:2]1([CH3:32])[C:6](=[O:7])[O:5][C:4]2[CH:8]=[CH:9][C:10]3[C:15]([C:3]1=2)=[CH:14][C:13]([CH:16](OS(C1C=CC(C)=CC=1)(=O)=O)[C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=3.[NH:33]1[CH:37]=[N:36][CH:35]=[N:34]1.O>S1(=O)(=O)CCCC1>[CH3:1][C:2]1([CH3:32])[C:6](=[O:7])[O:5][C:4]2[CH:8]=[CH:9][C:10]3[C:15]([C:3]1=2)=[CH:14][C:13]([CH:16]([N:33]1[CH:37]=[N:36][CH:35]=[N:34]1)[C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 92571H-1,2,4-TriazoleHCID 19858084HCID 19858084, 화합물

생성물 1

HCID 19858048HCID 19858048, 화합물

시약·촉매·용매 1

HCID 31347Sulfolane용매

실험 절차

A solution of 1,1-dimethyl-8-(2,2,2-trifluoro-1-tosyloxyethyl)-2(1H)-naphtho[2,1-b]furanone and 1,2,4-triazole (0.5 g) in tetrahydrothiophen-1,1-dioxide (1 ml) was heated at 140° for 18 h. The mixture was treated with water (20 ml) and extracted twice with diethyl ether, and the combined ether extracts were dried and evaporated to dryness under reduced pressure. The residue was purified by flash chromatography, using ethyl acetate: pentane, 1:1 v/v, as eluant, to give 1,1-dimethyl-8-[1-(1H-1,2,4-triazol-1-yl)-2,2,2-trifluoroethyl]-2(1H)-naphtho[2,1-b]furanone. Nmr in deuteriochloroform: δ 8.35(1H,s); 8.15(1H,d); 8.09(1H,s); 7.98(1H,d); 7.87(1H,d); 7.51(1H,dd); 7.46(1H,d); 6.14(1H,q); 1.78(3H,s); 1.75(3H,s).

후처리

  1. extractionextracted twice with diethyl ether
  2. dry with materialthe combined ether extracts were dried
  3. customevaporated to dryness under reduced pressure
  4. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-0970ef7bc4114b12b116ef4ad5ebdac8
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04916148

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