Hydrochloric Acid → HCID 22624532、化合物

HRID 279162ノート

反応式

HRID 279162 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[F:11][C:12]([F:30])([CH:27]([F:29])[F:28])[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([N:21]2[CH:25]=[N:24][NH:23][C:22]2=[O:26])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].Cl>C(OCC)(=O)C.O.CN(C)C=O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:23]2[C:22](=[O:26])[N:21]([C:18]3[CH:17]=[CH:16][C:15]([O:14][CH2:13][C:12]([F:11])([F:30])[CH:27]([F:28])[F:29])=[CH:20][CH:19]=3)[CH:25]=[N:24]2)=[CH:3][CH:4]=1)([O-:10])=[O:9]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 9590p-FluoronitrobenzeneHCID 11430Potassium CarbonateHCID 10779907HCID 10779907、化合物

生成物 1

HCID 22624532HCID 22624532、化合物収率 67%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4-fluoronitrobenzene (3.1 g), 4-[4-(2,2,3,3-tetrafluoropropoxy)phenyl]-3(2H,4H)-1,2,4-triazolone (5.8 g), potassium carbonate (13.8 g) and N,N-dimethylformamide (60 ml) was stirred at 80° C. for 2 hours. The resultant was cooled and poured into water (500 ml). The mixture was neutralized with hydrochloric acid and the precipitated crystals were collected by filtration. The crystals thus obtained were dissolved in ethyl acetate (300 ml) and dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue was crystallized from a mixture of ethyl acetate and diisopropyl ether to give 2-(4-nitrophenyl)-4-[4-(2,2,3,3-tetrafluoropropoxy)phenyl]-3(2H,4H)-1,2,4-triazolone (5.5 g, 67%) as yellow crystalline powders.

後処理

  1. temperatureThe resultant was cooled
  2. filtrationthe precipitated crystals were collected by filtration
  3. customThe crystals thus obtained
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe residue was crystallized from a mixture of ethyl acetate and diisopropyl ether

出典と根拠

ORDレコード
ord-5e0b21859aac456284c4c3aaa8c06614
出典データセット
uspto-grants-2002_03
特許番号
US06362206B1

反応ノート

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