Hydrochloric Acid → Ethyl Pyridazine-4-carboxylate

HRID 426267

反応式

HRID 426267 の反応式
Cl.[N:2]1[CH:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][N:3]=1.[CH2:11](O)[CH3:12]>>[CH2:11]([O:9][C:8]([C:5]1[CH:6]=[CH:7][N:2]=[N:3][CH:4]=1)=[O:10])[CH3:12]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 2761046Pyridazine-4-carboxylic Acid

生成物 1

HCID 10855652Ethyl Pyridazine-4-carboxylate収率 49%

実験手順

In a 250 mL round bottom flask, 1 mL concentrated HCl and 70 mL ethanol was added to pyridazine-4-carboxylic acid (3.78 g, 30.4 mmol). The mixture was refluxed overnight. The reaction was 80% complete based on HPLC. The reaction mixture was concentrated down. The residue was purified (silica gel, 2-10% MeOH/DCM) to give light yellow oil (1.8 g, 49%). 1H NMR (300 MHz, CD3OD): δ 9.62 (s, 1H), 9.43 (d, 1H), 8.08 (d, 1H), 4.52 (dd, 2H), 1.43 (t, 3H).

後処理

  1. temperatureThe mixture was refluxed overnight
  2. concentrationThe reaction mixture was concentrated down
  3. customThe residue was purified (silica gel, 2-10% MeOH/DCM)

出典と根拠

ORDレコード
ord-16f1bb33b8a148a9b6ca529f0525bc89
出典データセット
uspto-grants-2012_01
特許番号
US08106064B2

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