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

HRID 35333ノート

反応式

HRID 35333 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-381c5c99556c4f848281c9ccb2896c0f
出典データセット
uspto-grants-1988_08
特許番号
US04766125

反応ノート

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