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

HRID 1108838ノート

反応式

HRID 1108838 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aadc3dee1db2438e91674180470d596e
出典データセット
uspto-grants-2000_05
特許番号
US06069157

反応ノート

読み込み中…