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Dimethylformamide → 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methyl-N-(1-pyrazolyl)benzoic acid amide

HRID 1187951
ノート
印刷プレビュー

反応式

HRID 1187951 の反応式
CN(C)C=O.[NH2:6][N:7]1[CH:11]=[CH:10][CH:9]=[N:8]1.[Cl:12][C:13]1[CH:14]=[C:15]([C:20]2([C:35]([F:38])([F:37])[F:36])[O:24][N:23]=[C:22]([C:25]3[CH:33]=[CH:32][C:28]([C:29](Cl)=[O:30])=[C:27]([CH3:34])[CH:26]=3)[CH2:21]2)[CH:16]=[C:17]([Cl:19])[CH:18]=1.C(OCC)(=O)C>CN(C)C(=O)C>[Cl:12][C:13]1[CH:14]=[C:15]([C:20]2([C:35]([F:37])([F:36])[F:38])[O:24][N:23]=[C:22]([C:25]3[CH:33]=[CH:32][C:28]([C:29]([NH:6][N:7]4[CH:11]=[CH:10][CH:9]=[N:8]4)=[O:30])=[C:27]([CH3:34])[CH:26]=3)[CH2:21]2)[CH:16]=[C:17]([Cl:19])[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 118293521H-pyrazol-1-amineHCID 866114794-(5-(3,5-Dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl)-2-methylbenzoyl chloride

生成物 1

HCID 671639784-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methyl-N-(1-pyrazolyl)benzoic acid amide

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

In 4 mL of N,N-dimethylacetamide, 0.23 g of 50% N,N-dimethylformamide solution of 1-aminopyrazole was added, and 0.30 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methylbenzoyl-chloride synthesized in Step 4 of Synthetic Example 1 was added at room temperature with stirring, and stirred at the same temperature for 2 hours. After the completion of the reaction, 20 mL of ethyl acetate was added in the reaction mixture, washed with water (20 mL×1), and then the organic phase was dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with neutral alumina column chromatography that was eluated with chloroform to obtain 0.22 g of the aimed product as yellow resinous substance.

後処理

  1. stirringstirred at the same temperature for 2 hours
  2. additionwas added in the reaction mixture
  3. washwashed with water (20 mL×1)
  4. dry with materialdried over saturated sodium chloride aqueous solution
  5. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure
  6. customThe residue was purified with neutral alumina column chromatography that

出典と根拠

ORDレコード
ord-5e509835db1b444ca5d9a76fd09a87fe
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673951B2

反応ノート

読み込み中…

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