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

HRID 35329ノート

反応式

HRID 35329 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

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 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).

後処理

  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

出典と根拠

ORDレコード
ord-9a4a2ed6582a47a48d6db76908c0db46
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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