Water → HCID 178519429、化合物

HRID 25310

反応式

HRID 25310 の反応式
[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][NH:5][N:4]=1.[Cl:10][C:11]1[CH:18]=[C:17](F)[CH:16]=[CH:15][C:12]=1[CH:13]=[O:14].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:10][C:11]1[CH:18]=[C:17]([C:7]2[C:3]([C:2]([F:9])([F:8])[F:1])=[N:4][NH:5][CH:6]=2)[CH:16]=[CH:15][C:12]=1[CH:13]=[O:14]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1450242-Chloro-4-fluorobenzaldehydeHCID 18070343-(Trifluoromethyl)pyrazole

生成物 1

HCID 178519429HCID 178519429、化合物収率 550.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.08 g (30.0 mmol) of 3-trifluoromethylpyrazol, 4.75 mmol (30.0 mmol) of 2-chloro-4-fluorobenzaldehyde and 4.14 g (30.0 mmol) of potassium carbonate in 30 ml of N,N-dimethylformamide were stirred at 60° C. for 2 hours. After cooling to room temperature, the reaction mixture was poured into 100 ml of water, and the organic matters were extracted with 50 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. The residue afforded 7.18 g of 2-chloro-4-(3-trifluoromethylpyrazolyl)benzaldehyde (yield 87.2%) as a pale yellow powder, after washed with n-hexane.

後処理

  1. extractionthe organic matters were extracted with 50 ml of ethyl acetate twice
  2. washwashed with 50 ml of water twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe ethyl acetate was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-aef1a357148a4a72b8b8de7e3b3f270c
出典データセット
uspto-grants-2005_02
特許番号
US06858639B2

関連ノート

読み込み中…