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Tert-Butyl nitrite → HCID 9887618, 화합물

HRID 1108839
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HRID 1108839 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-6c1ca3cd8fd04244ad5965c943fe9eb2
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06069157

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