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Tert-Butyl nitrite → HCID 9887618, 화합물

HRID 1274362
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HRID 1274362 반응식
N[C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]#[N:20])[C:3]=1[C:21]1[CH:25]=[CH:24][O:23][C:22]=1[Cl:26].N(OC(C)(C)C)=O>O1CCCC1>[Cl:26][C:22]1[O:23][CH:24]=[CH:25][C:21]=1[C:3]1[C:4]([C:19]#[N:20])=[N:5][N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:15])[F:16])=[CH:9][C:8]=2[Cl:18])[CH:2]=1
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참가 물질

4

반응물 2

HCID 10906Tert-Butyl nitriteHCID 221209155-Amino-4-(2-chlorofuran-3-yl)-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole

생성물 1

HCID 9887618HCID 9887618, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
65 °C

실험 절차

To a solution of 5-amino-4-(2-chlorofuran-3-yl)-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole (0.204 g) in tetrahydrofuran (3 ml) was added t-butyl nitrite (171.8 μl). The mixture was heated to 65° C. for 1 hour, then cooled and evaporated. The residue was purified by column chromatography on silica gel (10 g) eluted with hexane containing increasing amounts of dichloromethane (up to 100%). Combination and evaporation of appropriate fraction gave the title compound as a white solid, m.p. 125° C.

후처리

  1. temperaturecooled
  2. customevaporated
  3. customThe residue was purified by column chromatography on silica gel (10 g)
  4. washeluted with hexane containing
  5. temperatureincreasing amounts of dichloromethane (up to 100%)
  6. customCombination and evaporation of appropriate fraction

출처 및 근거

ORD 기록
ord-49409b4237ab473c9117c039ac4a6c9e
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06156782

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