Oxygen → N-t-butoxycarbonyl-N-(2-oxo-ethyl)-2-phenyl-ethylamine

HRID 356861노트

반응식

HRID 356861 반응식
[C:1]([O:5][C:6]([N:8]([CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:9][CH:10]=C)=[O:7])([CH3:4])([CH3:3])[CH3:2].[O:20]=O.CSC>ClCCl.CO.C(OCC)(=O)C>[C:1]([O:5][C:6]([N:8]([CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:9][CH:10]=[O:20])=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

7

반응물 3

HCID 977OxygenHCID 1068Dimethyl SulfideHCID 53637355N-allyl-N-phenethylcarbamic acid tert-butyl ester

생성물 1

HCID 23225807N-t-butoxycarbonyl-N-(2-oxo-ethyl)-2-phenyl-ethylamine

시약·촉매·용매 3

HCID 887Methanol용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

반응 조건

온도
-78 °C

실험 절차

Dissolve N-t-butoxycarbonyl-N-allyl-2-phenyl-ethylamine (7.88 g, 21.44 mmol) in dichloromethane (200 mL) and methanol (5 mL). Cool to -78° C. Pass ozonized oxygen through the solution until a persistent light blue color is obtained. Pass nitrogen through the solution until the blue color dissipates. Add dimethyl sulfide (20 mL). Allow the reaction mixture to warm to ambient temperature and stir for 5 hours. Concentrate in vacuo to obtain a residue. Dilute the residue with ethyl acetate and extract with water. Separate the layers, dry the organic layer over MgSO4, filter, and evaporate in vacuo to give the title compound.

후처리

  1. customis obtained
  2. temperatureto warm to ambient temperature
  3. concentrationConcentrate in vacuo
  4. customto obtain a residue
  5. extractionextract with water
  6. customSeparate the layers
  7. dry with materialdry the organic layer over MgSO4
  8. filtrationfilter
  9. customevaporate in vacuo

출처 및 근거

ORD 기록
ord-001047ccd7914986a2b6c586054ecd09
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840726

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