Tert-Butyl nitrite → 3-Cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole

HRID 1108838노트

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HRID 1108838 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][CH:22]=1.N(OC(C)(C)C)=O>O1CCCC1>[C:19]([C:4]1[C:3]([C:21]2[CH:25]=[CH:24][O:23][CH:22]=2)=[CH:2][N:6]([C:7]2[C:8]([Cl:18])=[CH:9][C:10]([C:14]([F:17])([F:15])[F:16])=[CH:11][C:12]=2[Cl:13])[N:5]=1)#[N:20]

참가 물질

4

반응물 2

HCID 10906Tert-Butyl nitriteHCID 221209065-Amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(3-furanyl)pyrazole

생성물 1

HCID 221208903-Cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
65 °C

실험 절차

To a solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole (0.204 g) in tetrahydrofuran (3 ml) was added t-butyl nitrite (187.8 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 (5 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. 139° C.

후처리

  1. temperaturecooled
  2. customevaporated The residue
  3. customwas purified by column chromatography on silica gel (5 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-aadc3dee1db2438e91674180470d596e
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06069157

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