Sodium Acetate → HCID 90029515、化合物

HRID 1488214ノート

反応式

HRID 1488214 の反応式
[CH2:1]([N:8]1[CH:12]=[C:11]([CH3:13])[C:10]([CH2:14][OH:15])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1C=C[NH+]=CC=1.C1C=C[NH+]=CC=1.[O-][Cr](O[Cr]([O-])(=O)=O)(=O)=O.CC([O-])=O.[Na+]>ClCCl>[CH2:1]([N:8]1[CH:12]=[C:11]([CH3:13])[C:10]([CH:14]=[O:15])=[N:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 517045Sodium AcetateHCID 2724130Cornforth reagentHCID 90029703HCID 90029703、化合物2 回

生成物 1

HCID 90029515HCID 90029515、化合物収率 34%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (1-benzyl-4-methyl-1H-pyrazol-3-yl)methanol (compound 268.2, 3 g, 14.8 mmol) in dichloromethane (100 mL) was added PDC (11.3 g, 30.1 mmol), molecular sieves (3 g) and NaOAc (300 mg) were added to the reaction mixture. The reaction mixture was stirred for 4 h at room temperature. The solids were removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by a silica gel chromatography with ethyl acetate/petroleum ether (1/10) as the eluent to yield 1 g (34%) of the title compound as a colorless oil.

後処理

  1. additionwere added to the reaction mixture
  2. customThe solids were removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by a silica gel chromatography with ethyl acetate/petroleum ether (1/10) as the eluent

出典と根拠

ORDレコード
ord-6ad90c0235444c9984e1a5df83c78768
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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