Acetohydrazide → HCID 178493714, 화합물

HRID 1394452노트

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HRID 1394452 반응식
COC1C=[N:10][C:9]([C:12]#[N:13])=[C:8]2[C:4]=1[CH:5]=[CH:6][NH:7]2.[C:14]([NH:17][NH2:18])(=O)[CH3:15].[CH2:19]([O:21][C:22]([CH3:24])=O)C.O>>[CH3:19][O:21][C:22]1[CH:24]=[N:10][C:9]([C:12]2[NH:13][C:14]([CH3:15])=[N:17][N:18]=2)=[C:8]2[C:4]=1[CH:5]=[CH:6][NH:7]2

참가 물질

4

반응물 3

HCID 14039AcetohydrazideHCID 22728543Water ethylacetateHCID 450911364-Methoxy-1H-pyrrolo[2,3-c]pyridine-7-carbonitrile

생성물 1

HCID 178493714HCID 178493714, 화합물수율 26%

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온도
150 °C

실험 절차

A mixture of 4-methoxy-7-cyano-6-azaindole (0.131 g, 0.757 mmol) and acetic hydrazide (0.270 g, 3.645 mmol) was heated in a sealed tube at 150° C. for 48 h. The reaction mixture was cooled and the solid residue was diluted with EtOAc-H2O. The aqueous phase was separated and re-extracted twice with EtOAc. The combined organic layers were washed (H2O, brine), dried (Na2SO4) and concentrated, and the residue was purified by preparative HPLC (NH4OAc), affording the title compound (0.0455 g, 26%) as a colorless solid:

후처리

  1. temperatureThe reaction mixture was cooled
  2. customThe aqueous phase was separated
  3. extractionre-extracted twice with EtOAc
  4. washThe combined organic layers were washed (H2O, brine)
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customthe residue was purified by preparative HPLC (NH4OAc)

출처 및 근거

ORD 기록
ord-33af9e05e1614e2bb65af96c497fe89a
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07348337B2

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