Triethylamine → N-(5-fluoro-2-methylphenyl)-tetrahydro-3,3-dimethyl-3H-oxazolo[3,4-a]pyrazine-7(8H)-acetamide

HRID 35333노트

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HRID 35333 반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:7]=1[CH3:13])=[O:4].[CH3:14][C:15]1([CH3:24])[N:19]2[CH2:20][CH2:21][NH:22][CH2:23][CH:18]2[CH2:17][O:16]1.C(N(CC)CC)C>CN(C)C=O>[F:12][C:10]1[CH:9]=[CH:8][C:7]([CH3:13])=[C:6]([NH:5][C:3](=[O:4])[CH2:2][N:22]2[CH2:21][CH2:20][N:19]3[C:15]([CH3:24])([CH3:14])[O:16][CH2:17][CH:18]3[CH2:23]2)[CH:11]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 7358522-chloro-N-(5-fluoro-2-methylphenyl)acetamideHCID 212956453,3-Dimethylhexahydro-3H-[1,3]oxazolo[3,4-a]pyrazine

생성물 1

HCID 21295689N-(5-fluoro-2-methylphenyl)-tetrahydro-3,3-dimethyl-3H-oxazolo[3,4-a]pyrazine-7(8H)-acetamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

A mixture of 6.6 parts of 2-chloro-N-(5-fluoro-2-methylphenyl)acetamide, 5 parts of hexahydro-3,3-dimethyl-3H-oxazolo[3,4-a]pyrazine, 6.1 parts of N,N-diethylethanamine and 67.5 parts of N,N-dimethylformamide was stirred and heated for 8 hours at about 70° C. After cooling overnight to room temperature, the reaction mixture was evaporated. The residue was dissolved in trichloromethane. The solution was washed with water, dried, filtered and evaporated, yielding 8.5 parts of N-(5-fluoro-2-methylphenyl)-tetrahydro-3,3-dimethyl-3H-oxazolo[3,4-a]pyrazine-7(8H)-acetamide as an oily residue (intermediate 121).

후처리

  1. temperatureAfter cooling overnight to room temperature
  2. customthe reaction mixture was evaporated
  3. dissolutionThe residue was dissolved in trichloromethane
  4. washThe solution was washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-381c5c99556c4f848281c9ccb2896c0f
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766125

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