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

HRID 377664ノート

反応式

HRID 377664 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7c09078dd64c4beca4c39a7f7edeabe0
出典データセット
uspto-grants-2000_02
特許番号
US06028096

反応ノート

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