Ethanol → HCID 22605344、化合物

HRID 241945ノート

反応式

HRID 241945 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 22605344HCID 22605344、化合物

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb6ab8a4eed7468b98a5a508a2f53c11
出典データセット
uspto-grants-2014_02
特許番号
US08653097B2

反応ノート

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