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Acetic Acid → HCID 67351373, 화합물

HRID 910578
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HRID 910578 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 67351373HCID 67351373, 화합물수율 75.2%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6c8919b9d9dc48b1b5205db9c9aadbc3
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022192B2

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