Formic Acid → HCID 23117566、化合物

HRID 1178325ノート

反応式

HRID 1178325 の反応式
[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]

参加物

5

反応物 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 23117571HCID 23117571、化合物

生成物 1

HCID 23117566HCID 23117566、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5ff0d1252e8746db844a9e7671c7df61
出典データセット
uspto-grants-2007_10
特許番号
US07276511B2

反応ノート

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