Sodium Acetate → HCID 90029515, 화합물

HRID 1488214노트

반응식

HRID 1488214 반응식
[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

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 2724130Cornforth reagentHCID 90029703HCID 90029703, 화합물2회

생성물 1

HCID 90029515HCID 90029515, 화합물수율 34%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ad90c0235444c9984e1a5df83c78768
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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