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Water → HCID 67350623, 화합물

HRID 910581
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HRID 910581 반응식
[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.[CH2:17]([O:24][C:25](ON1C(=O)CCC1=O)=[O:26])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O.C(OCC)(=O)C>CN(C)C=O>[CH2:17]([O:24][C:25]([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:26])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
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참가 물질

6

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HCID 962WaterHCID 8857Ethyl AcetateHCID 83172Benzyl succinimido carbonateHCID 673516914-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one

생성물 1

HCID 67350623HCID 67350623, 화합물수율 35.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

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온도
50 °C

실험 절차

4-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (2.00 g) was dissolved in N,N-dimethylformamide (5 mL) at room temperature. N-(Benzyloxycarbonyloxy)succinimide (2.42 g) was added to the solution. The mixture was heated to 50° C. and then stirred for 16 hours. After the addition of water (20 mL) and ethyl acetate (20 mL) to the reaction mixture, the aqueous layer was separated, and the organic layer was washed with water. The obtained organic layer was concentrated under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: ethyl acetate/dichloromethane=1/3 to 1/1) to give 1-benzyloxycarbonyl-4-benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (1.15 g).

후처리

  1. customthe aqueous layer was separated
  2. washthe organic layer was washed with water
  3. concentrationThe obtained organic layer was concentrated under reduced pressure
  4. customthe residue was purified by column chromatography on silica gel (eluent: ethyl acetate/dichloromethane=1/3 to 1/1)

출처 및 근거

ORD 기록
ord-16a0481e1f3b4006939cdd3a796770e7
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022192B2

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