Dimethylformamide → HCID 178421927, 화합물

HRID 503748

반응식

HRID 503748 반응식
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

참가 물질

7

반응물 3

HCID 6228DimethylformamideHCID 95389Ethyl acetylphenylacetateHCID 178418311HCID 178418311, 화합물

생성물 1

HCID 178421927HCID 178421927, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 7622Tributylamine용매

반응 조건

온도
180 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-637348febe354317b72ed4226981a1e6
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776864B2

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