Bentonite → HCID 178425431、化合物

HRID 20320

反応式

HRID 20320 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[C:15]([NH2:16])=[CH:14][NH:13][N:12]=2)=[O:10])=[CH:4][CH:3]=1.O.[O-2].[O-2].[O-2].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.[Al+3].[Al+3]>C(CC(=O)C)C(C)=O.CO.ClCCl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[C:15]([N:16]3[C:4]([CH3:5])=[CH:3][CH:2]=[C:7]3[CH3:6])=[CH:14][NH:13][N:12]=2)=[O:10])=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 71586775BentoniteHCID 178508056HCID 178508056、化合物

生成物 1

HCID 178425431HCID 178425431、化合物

試薬・触媒・溶媒 2

HCID 80352,5-Hexanedione溶媒HCID 21226129Dichloromethane methanol溶媒

反応条件

温度
120 °C

実験手順

A mixture of 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (100 mg) and Montmorillonite KSF clay (100 mg) in acetonylacetone (1 ml) was heated at 120° C. (50 W) for 15 minutes in a CEM discover microwave synthesiser. The reaction mixture was diluted with 5% methanol/dichloromethane, filtered and evaporated. The crude product was purified by flash column chromatography eluting with 1:2 ethyl acetate/hexane, and the product containing fractions were combined and evaporated to give 65 mg of the target molecule as a pale brown solid. (LC/MS: Rt 3.75 [M+H]+ 299).

後処理

  1. filtrationfiltered
  2. customevaporated
  3. customThe crude product was purified by flash column chromatography
  4. washeluting with 1:2 ethyl acetate/hexane
  5. additionthe product containing fractions
  6. customevaporated
  7. customto give 65 mg of the target molecule as a pale brown solid

出典と根拠

ORDレコード
ord-aa3be304f8654d67b5c9d429009d1f72
出典データセット
uspto-grants-2010_06
特許番号
US07745638B2

関連ノート

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