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2-(Benzenesulfonyl)-3-phenyloxaziridine → HCID 68858127, 화합물

HRID 1783534
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HRID 1783534 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:11]2[CH2:20][C:19]3[C:14](=[N:15][C:16]([S:21][CH3:22])=[N:17][CH:18]=3)[N:13]([CH2:23][CH3:24])[C:12]2=[O:25])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.C1(C2[O:34]N2S(C2C=CC=CC=2)(=O)=O)C=CC=CC=1>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:11]2[CH2:20][C:19]3[C:14](=[N:15][C:16]([S:21]([CH3:22])=[O:34])=[N:17][CH:18]=3)[N:13]([CH2:23][CH3:24])[C:12]2=[O:25])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3204052-(Benzenesulfonyl)-3-phenyloxaziridineHCID 688614513-(3,5-Dimethoxyphenyl)-1-ethyl-7-(methylsulfanyl)-3,4-dihydropyrimido[4,5-D]pyrimidin-2(1H)-one

생성물 1

HCID 68858127HCID 68858127, 화합물수율 78.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-(3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfanyl-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one (5.61 g, 15.57 mmol) in dichloromethane (100 mL) at ambient temperature was added 3-phenyl-2-(phenylsulfonyl)oxaziridine (4.88 g, 18.69 mmol, PD 0191006, Org. Synth., 1987; 66:203-210) in portions. The reaction mixture was stirred overnight, then washed with brine and water. The organic layer was dried over magnesium sulfate, filtered, and evaporated under reduced pressure. The residue was purified by column chromatography eluting with a solvent mixture of 3% methanol in dichloromethane to yield 4.6 g (78%) of the titled compound: mp 167-169° C. Mass Spectrum (APCI, 80/20 CH3CN/H2O, Probe=450° C.) (m+1)/z 377.1

후처리

  1. washwashed with brine and water
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe residue was purified by column chromatography
  6. washeluting with a solvent mixture of 3% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-1fc1d0f6e1a44b70bf9dc9cc9623396a
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07501425B1

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