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Water → HCID 9878958, 화합물

HRID 642098
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HRID 642098 반응식
[O:1]([CH2:8][C:9]([NH:11][C:12]1[CH:21]=[CH:20][C:15]([C:16](OC)=[O:17])=[CH:14][CH:13]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:23][NH2:24].O>CCO>[NH:23]([C:16]([C:15]1[CH:20]=[CH:21][C:12]([NH:11][C:9](=[O:10])[CH2:8][O:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:13][CH:14]=1)=[O:17])[NH2:24]
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참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 674765HCID 674765, 화합물

생성물 1

HCID 9878958HCID 9878958, 화합물수율 46%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of methyl 4-[(phenoxyacetyl)amino]benzoate (843 mg, 2.95 mmol) in EtOH (10 mL) was added hydrazine hydrate (2.15 mL). After stirring for 15 hrs at reflux, the reaction mixture was cooled to rt. Water (10 mL) was added to the reaction mixture and a white solid precipitated out. Filtration, washing with EtOH/water (2×2 mL) and water (3×1 mL), and drying under vacuo at 70° C. for 6 hrs gave 389 mg of the title compound (46%) as a white solid in 95.4% purity by HPLC (MaxPlot detection between 230 and 400 nm).

후처리

  1. temperatureat reflux
  2. customa white solid precipitated out
  3. filtrationFiltration
  4. washwashing with EtOH/water (2×2 mL) and water (3×1 mL)
  5. customdrying under vacuo at 70° C. for 6 hrs

출처 및 근거

ORD 기록
ord-f65e0f7b19d04c81b4b6d186e249c5da
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07696231B2

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