Piperidine → 2,6-Dimethyl-1-oxo-4-(piperidin-1-yl)-1lambda~5~-pyrimidine

HRID 1755652ノート

反応式

HRID 1755652 の反応式
[CH3:1][C:2]1[N+:7]([O-:8])=[C:6]([CH3:9])[CH:5]=[C:4](Cl)[N:3]=1.[NH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1>>[CH3:1][C:2]1[N+:7]([O-:8])=[C:6]([CH3:9])[CH:5]=[C:4]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:3]=1

参加物

3

反応物 2

HCID 8082PiperidineHCID 126992254-Chloro-2,6-dimethylpyrimidine 1-oxide

生成物 1

HCID 157346332,6-Dimethyl-1-oxo-4-(piperidin-1-yl)-1lambda~5~-pyrimidine

実験手順

100 ml of piperidine are introduced into a 250 ml three-necked flask fitted with a thermometer, a condenser and a magnetic stirrer and 13.5 g (8.51×10-2 mol) of 2,4-dimethyl-6-chloropyrimidine 3-oxide are then added, in solid portions, in a manner such that exothermic heat does not develop beyond 60° C. The reaction mixture is then allowed to return to ambient temperature; the piperidinium hydrochloride is then removed from the mixture by filtration and the filtrate is evaporated to dryness. The crude oil obtained crystallises rapidly at ambient temperature. The crystalline mass is dissolved in a minimum of ethanol and ethyl ether is then added cold until precipitation occurs. The mixture is stirred for half an hour and the precipitate is then filtered off and drained. A final filtration through silica gel using the dichloromethane/methanol (90/10) eluent system allows white crystals to be obtained.

後処理

  1. additionare then added, in solid portions, in a manner such
  2. temperaturethat exothermic heat
  3. customdoes not develop beyond 60° C
  4. customto return to ambient temperature
  5. customthe piperidinium hydrochloride is then removed from the mixture by filtration
  6. customthe filtrate is evaporated to dryness
  7. customThe crude oil obtained
  8. customcrystallises rapidly at ambient temperature
  9. dissolutionThe crystalline mass is dissolved in a minimum of ethanol and ethyl ether
  10. additionis then added cold
  11. customuntil precipitation
  12. filtrationthe precipitate is then filtered off
  13. filtrationA final filtration through silica gel using the dichloromethane/methanol (90/10) eluent system
  14. customto be obtained

出典と根拠

ORDレコード
ord-a7065a85d24549febaebe0ffc4b66cfa
出典データセット
uspto-grants-1995_08
特許番号
US05438058

反応ノート

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