Methyl iodide → 1,6-Dimethyluracil

HRID 1744761ノート

反応式

HRID 1744761 の反応式
C[O:2][C:3]1[N:8]=[C:7]([O:9]C)[CH:6]=[C:5]([CH3:11])[N:4]=1.I[CH3:13]>>[CH3:13][N:4]1[C:5]([CH3:11])=[CH:6][C:7](=[O:9])[NH:8][C:3]1=[O:2]

参加物

3

反応物 2

HCID 6328Methyl iodideHCID 2698202,4-Dimethoxy-6-methylpyrimidine

生成物 1

HCID 106068181,6-Dimethyluracil

実験手順

14.2 g (92 mmol) 2,4-dimethoxy-6-methylpyrimidine was dissolved in 210 mL iodomethane and the reaction allowed to continue for 2 days at room temperature. After 2 days, the excess of iodomethane was evaporated off under reduced pressure, the residue treated with 675 mL 1 N HCl and the resulting mixture refluxed for one and a half hours. After cooling to room temperature and neutralization with a concentrated sodium hydroxide solution, the water was removed under reduced pressure and the residue extracted with chloroform using a Soxhlet extractor. The chloroform was evaporated under reduced pressure and the crude compound recrystallized first from ethanol and then from water yielding 4.03 g (31%) of 1,6-dimethyluracil (m.p. 221–223° C.).

後処理

  1. waitAfter 2 days
  2. customthe excess of iodomethane was evaporated off under reduced pressure
  3. additionthe residue treated with 675 mL 1 N HCl
  4. temperaturethe resulting mixture refluxed for one and a half hours
  5. customneutralization with a concentrated sodium hydroxide solution, the water was removed under reduced pressure
  6. extractionthe residue extracted with chloroform using a Soxhlet extractor
  7. customThe chloroform was evaporated under reduced pressure
  8. customthe crude compound recrystallized first from ethanol

出典と根拠

ORDレコード
ord-489c6aef5e3e4f18b579717bd0152198
出典データセット
uspto-grants-2006_03
特許番号
US07018786B2

反応ノート

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