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Ethanol → HCID 2836660, 화합물

HRID 535536
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HRID 535536 반응식
[C:1]([CH:4]([C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9](=[O:16])[NH:8][N:7]=1)[CH3:5])([OH:3])=[O:2].S(Cl)(Cl)=O.[CH3:21][CH2:22]O>>[O:16]=[C:9]1[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:6]([CH:4]([CH3:5])[C:1]([O:3][CH2:21][CH3:22])=[O:2])=[N:7][NH:8]1
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참가 물질

4

반응물 3

HCID 702EthanolHCID 24386Thionyl ChlorideHCID 28366592-(4-Oxo-3,4-dihydrophthalazin-1-yl)propanoic acid

생성물 1

HCID 2836660HCID 2836660, 화합물

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온도
80 °C

실험 절차

To a solution of 4-(1-carboxyethyl)-1(2H)-phthalazinone (1.5 g, 6.9 mmol) in EtOH (50 mL) was added thionyl chloride (1.10 mL, 15.1 mmol). The mixture was stirred at 80° C. for 4 hours, cooled to 0° C., and quenched with 1M NaHCO3 (40 mL). The aq layer was extracted with EtOAc (2×50 mL), dried (Na2SO4), filtered, and concentrated to give the title compound: MS (ESI+) M/Z 247 (M+H)+.

후처리

  1. temperaturecooled to 0° C.
  2. customquenched with 1M NaHCO3 (40 mL)
  3. extractionThe aq layer was extracted with EtOAc (2×50 mL)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0c7a2e438115449098e3a414a15d7fed
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859549B2

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