Acetic Acid → HCID 178470180、化合物

HRID 1108860ノート

反応式

HRID 1108860 の反応式
C([NH:3][C:4](=O)[C:5]([O-:7])=S)C.Cl.[NH2:10][CH2:11][C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=O.[C:20]([O-])(=O)[CH3:21].[Na+].C(O)(=[O:27])C>>[C:14]1([C:12]2[N:3]=[C:4]([C:5]([O:7][CH2:20][CH3:21])=[O:27])[NH:10][CH:11]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 4

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 2723597Ethanone, 2-amino-1-phenyl-, hydrochloride (1:1)HCID 178465254HCID 178465254、化合物

生成物 1

HCID 178470180HCID 178470180、化合物

実験手順

A mixture of 3 g of ethylthiooxamate, 4.25 g of 2-aminoacetophenone hydrochloride and 3.69 g of sodium acetate was dissolved in 20 mL of acetic acid and heated under reflux for 3 hr. The reaction mixture was allowed to cool to room temperature and the acetic acid removed by evaporation under reduced pressure. The residue was basified with aqueous sodium carbonate and extracted with 2×100 mL of ethyl acetate. The combined extracts were washed with 2×100 mL of brine, dried over anhydrous sodium sulfate and the solvent removed under reduced pressure to yield 2.8 g of ethyl 4-phenylimidazole-2-carboxylate as a solid which was used in the next step without further purification or characterization.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 3 hr
  3. customthe acetic acid removed by evaporation under reduced pressure
  4. extractionextracted with 2×100 mL of ethyl acetate
  5. washThe combined extracts were washed with 2×100 mL of brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-83d300c2383948b3beb3765e2b89b22c
出典データセット
uspto-grants-2000_05
特許番号
US06069251

反応ノート

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