Dimethylformamide → HCID 178421927、化合物

HRID 503748

反応式

HRID 503748 の反応式
N1[CH:5]=[N:4][C:3]([NH2:6])=[N:2]1.O=[C:8]([CH3:21])[CH:9]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:10](OCC)=[O:11].[CH3:22]N(C=O)C>C(N(CCCC)CCCC)CCC.O.ClCCl>[CH3:21][C:8]1[N:6]2[CH:22]=[CH:5][N:4]=[C:3]2[N:2]=[C:10]([OH:11])[C:9]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

7

反応物 3

HCID 6228DimethylformamideHCID 95389Ethyl acetylphenylacetateHCID 178418311HCID 178418311、化合物

生成物 1

HCID 178421927HCID 178421927、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 7622Tributylamine溶媒

反応条件

温度
180 °C

実験手順

A solution of 3.8 g 1,2,4-triazol-3-amine and 6 g ethyl 3-oxo-2-phenylbutanoate is suspended in a mixture of 32 ml DMF and 32 ml N,N-dibutylbutan-1-amine and heated by microwave irradiation to 180° C. for 10 h. The reaction mixture is diluted with water and dichloromethane, the phases separated, the aqueous layer extracted twice with dichloromethane, the combined organic layers are dried over Na2SO4 and concentrated to give the crude product. The crude product is purified by column chromatography (silica gel, dichloromethane/methanol).

後処理

  1. customthe phases separated
  2. extractionthe aqueous layer extracted twice with dichloromethane
  3. dry with materialthe combined organic layers are dried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-637348febe354317b72ed4226981a1e6
出典データセット
uspto-grants-2010_08
特許番号
US07776864B2

関連ノート

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