Ethanol → HCID 22605344, 화합물

HRID 241945노트

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HRID 241945 반응식
[O:1]=[C:2]1[CH2:7][CH2:6][CH2:5][N:4]2[N:8]=[C:9]([C:11]([OH:13])=[O:12])[CH:10]=[C:3]12.S(=O)(=O)(O)O.[CH3:19][CH2:20]O>>[CH2:19]([O:12][C:11]([C:9]1[CH:10]=[C:3]2[C:2](=[O:1])[CH2:7][CH2:6][CH2:5][N:4]2[N:8]=1)=[O:13])[CH3:20]

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 226053224-oxo-4H,5H,6H,7H-pyrazolo[1,5-a]pyridine-2- carboxylic acid

생성물 1

HCID 22605344HCID 22605344, 화합물

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온도
100 °C

실험 절차

To a mixture of 4-oxo-4,5,6,7-tetrahydro-pyrazolo[1,5-a]pyridine-2-carboxylic acid (16 g, 89 mmol) in 170 mL EtOH is added slowly 12 mL concentrated sulphuric acid and the reaction mixture is heated to 100° C. for 2 h. The reaction mixture is cooled to RT and concentrated under reduced pressure. The residue is poured on ice, neutralized by the addition of an aqueous saturated solution of NaHCO3 and extracted with DCM. The combined organic phases are washed with water and brine, dried on MgSO4 and the solvent are removed under reduced pressure. Yield: 17 g. HPLC-MS: Rt=1.79 min, (M+H)+=209.

후처리

  1. temperatureThe reaction mixture is cooled to RT
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue is poured on ice
  4. additionneutralized by the addition of an aqueous saturated solution of NaHCO3
  5. extractionextracted with DCM
  6. washThe combined organic phases are washed with water and brine
  7. customdried on MgSO4
  8. customthe solvent are removed under reduced pressure

출처 및 근거

ORD 기록
ord-bb6ab8a4eed7468b98a5a508a2f53c11
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653097B2

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