Sodium Carbonate → 7-[4,4-bis(4-fluorophenyl)butyl]hexahydro-3,3-dimethyl-1H-oxazolo[3,4-a]pyrazine

HRID 35329노트

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HRID 35329 반응식
I[CH2:2][CH2:3][CH2:4][CH:5]([C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=1)[C:6]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][CH:7]=1.[CH3:20][C:21]1([CH3:30])[N:25]2[CH2:26][CH2:27][NH:28][CH2:29][CH:24]2[CH2:23][O:22]1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[F:12][C:9]1[CH:10]=[CH:11][C:6]([CH:5]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[CH2:4][CH2:3][CH2:2][N:28]2[CH2:27][CH2:26][N:25]3[C:21]([CH3:30])([CH3:20])[O:22][CH2:23][CH:24]3[CH2:29]2)=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 1039681,1'-(4-Iodobutylidene)bis[4-fluorobenzene]HCID 212956453,3-Dimethylhexahydro-3H-[1,3]oxazolo[3,4-a]pyrazine

생성물 1

HCID 212957107-[4,4-bis(4-fluorophenyl)butyl]hexahydro-3,3-dimethyl-1H-oxazolo[3,4-a]pyrazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

A mixture of 30.7 parts of 1,1'-(4-iodobutylidene)bis[4-fluorobenzene], 11.5 parts of hexahydro-3,3-dimethyl-1H-oxazolo-[3,4-a]pyrazine, 14.8 parts of sodium carbonate and 270 parts of N,N-dimethylformamide was stirred for 5 hours at about 70° C. The reaction mixture was cooled overnight to room temperature and the solvent was evaporated. The residue was dissolved in trichloromethane. The organic phase was washed with water, dried, filtered and evaporated, yielding 34 parts of 7-[4,4-bis(4-fluorophenyl)butyl]hexahydro-3,3-dimethyl-1H-oxazolo[3,4-a]pyrazine as a residue (intermediate 94).

후처리

  1. temperatureThe reaction mixture was cooled overnight to room temperature
  2. customthe solvent was evaporated
  3. dissolutionThe residue was dissolved in trichloromethane
  4. washThe organic phase was washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-9a4a2ed6582a47a48d6db76908c0db46
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766125

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