Tert-Butyl nitrite → 4-Acetyl-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole

HRID 377664노트

반응식

HRID 377664 반응식
[C:1]([C:4]1[C:5]([C:23]#[N:24])=[N:6][N:7]([C:10]2[C:15]([Cl:16])=[CH:14][C:13]([O:17][C:18]([F:21])([F:20])[F:19])=[CH:12][C:11]=2[Cl:22])[C:8]=1N)(=[O:3])[CH3:2].C(ON=O)(C)(C)C>O1CCCC1>[C:1]([C:4]1[C:5]([C:23]#[N:24])=[N:6][N:7]([C:10]2[C:15]([Cl:16])=[CH:14][C:13]([O:17][C:18]([F:19])([F:21])[F:20])=[CH:12][C:11]=2[Cl:22])[CH:8]=1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 10906Tert-Butyl nitriteHCID 193564804-Acetyl-5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole

생성물 1

HCID 193564794-Acetyl-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 4-acetyl-5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethoxyphenyl)pyrazole (0.302 g) in tetrahydrofuran (10 ml) at 2° C. was added t-butylnitrite (0.66 ml). The mixture was heated under reflux for 1.5 hours and then evaporated. The residue was purified by column chromatography on silica gel eluted with dichloromethane. Combination and evaporation of suitable fractions provided the title compound as a white solid, m.p. 105.7-106.6° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. washeluted with dichloromethane
  6. customCombination and evaporation of suitable fractions

출처 및 근거

ORD 기록
ord-7c09078dd64c4beca4c39a7f7edeabe0
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06028096

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