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Acetic Acid → HCID 67351373、化合物

HRID 910578
ノート
印刷プレビュー

反応式

HRID 910578 の反応式
[CH2:1]([C:8]1[C:9](=[O:14])[NH:10][NH:11][C:12]=1[CH3:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:21](OC(=O)C)(=[O:23])[CH3:22].C(O)(=O)C>CN(C)C=O.O>[C:21]([N:11]1[C:12]([CH3:13])=[C:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:9](=[O:14])[NH:10]1)(=[O:23])[CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 69228064-Benzyl-1,2-dihydro-5-methyl-3H-pyrazol-3-one

生成物 1

HCID 67351373HCID 67351373、化合物収率 75.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

4-Benzyl-1,2-dihydro-5-methyl-3H-pyrazol-3-one (1.00 g) was suspended in N,N-dimethylformamide (5 mL) at room temperature. In addition, potassium carbonate (0.441 g) was added to the suspension, and the mixture was stirred for 30 minutes. Acetic anhydride (0.570 g) was added to the mixture in a dropwise manner at room temperature. The mixture was stirred at room temperature overnight and at 50° C. for 2 hours. In addition, the mixed solution of glacial acetic acid (0.191 g) and water (5.0 g) was added to the reaction mixture under stirring at room temperature. After confirming the precipitation of the crystals, water (25 g) was added to the mixture under stirring. The crystals were collected by filtration, washed with water and dried under reduced pressure to give a white solid of 1-acetyl-4-benzyl-1,2-dihydro-5-methyl-3H-pyrazol-3-one (0.92 g).

後処理

  1. stirringThe mixture was stirred at room temperature overnight and at 50° C. for 2 hours
  2. stirringunder stirring at room temperature
  3. customthe precipitation of the crystals, water (25 g)
  4. additionwas added to the mixture
  5. stirringunder stirring
  6. filtrationThe crystals were collected by filtration
  7. washwashed with water
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6c8919b9d9dc48b1b5205db9c9aadbc3
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08022192B2

反応ノート

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