Formic Acid → HCID 23117566, 화합물

HRID 1178325노트

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HRID 1178325 반응식
[CH:1](O)=[O:2].C(OC(=O)C)(=O)C.[NH2:11][C:12]([C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([Cl:28])[CH:22]=1)([CH2:18][CH:19]=[CH2:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14]>O1CCCC1>[Cl:28][C:23]1[CH:22]=[C:21]([C:12]([NH:11][CH:1]=[O:2])([CH2:18][CH:19]=[CH2:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:26]=[CH:25][C:24]=1[Cl:27]

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 23117571HCID 23117571, 화합물

생성물 1

HCID 23117566HCID 23117566, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

Under cooling on ice, formic acid (140 mL) was added to acetic anhydride (255 mL), followed by stirring at 50° C. for 30 minutes. The reaction mixture was cooled with ice. Subsequently, ethyl 2-amino-2-(3,4-dichlorophenyl)-4-pentenoate (298 g) in tetrahydrofuran (1.5 L) was added to the mixture, and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was concentrated under reduced pressure. The residue was neutaralized with saturated aqueous sodium bicarbonate. The resultant mixture was subjected to extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate anhydrate. The solvent was removed under reduced pressure, to thereby give the title compound (334 g). The title compound was used in the next step without further purification.

후처리

  1. temperatureThe reaction mixture was cooled with ice
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. extractionThe resultant mixture was subjected to extraction with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over sodium sulfate anhydrate
  7. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-5ff0d1252e8746db844a9e7671c7df61
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07276511B2

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