Acetic Anhydride → HCID 67348858、化合物

HRID 910577ノート

反応式

HRID 910577 の反応式
[CH2:1]([C:8]1[C:9](=[O:16])[NH:10][NH:11][C:12]=1[CH:13]([CH3:15])[CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>O1CCCC1.C(O)(=O)C>[C:17]([N:11]1[C:12]([CH:13]([CH3:14])[CH3:15])=[C:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:9](=[O:16])[NH:10]1)(=[O:19])[CH3:18]

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 673516914-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one

生成物 1

HCID 67348858HCID 67348858、化合物収率 77%

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒HCID 8028Tetrahydrofuran溶媒

実験手順

4-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (1.50 g) was dissolved in tetrahydrofuran (6.0 g) at room temperature. Acetic anhydride (0.708 g) and acetic acid (0.0208 g) was added to the solution successively. After the reaction mixture was stirred at room temperature for 15 hours, the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (The product was eluted with dichloromethane at first, and then n-hexane/ethyl acetate=4/1) to give 1-acetyl-4-benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (1.38 g).

後処理

  1. customthe solvent was removed under reduced pressure
  2. customThe residue was purified by column chromatography on silica gel (The product
  3. washwas eluted with dichloromethane at first, and then n-hexane/ethyl acetate=4/1)

出典と根拠

ORDレコード
ord-579bd2bac8bb45139b4b49b6448392db
出典データセット
uspto-grants-2011_09
特許番号
US08022192B2

反応ノート

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