Acetic Acid → HCID 178470180, 화합물

HRID 2257299노트

반응식

HRID 2257299 반응식
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

참가 물질

5

반응물 4

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

생성물 1

HCID 178470180HCID 178470180, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d7dd7c24b680494a8d75b5c3807a17bb
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05656762

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