Urea, (3-methoxyphenethyl)- → 1-[2-(3-Methoxyphenyl)ethyl]pyrimidine-2,4,6(1H,3H,5H)-trione

HRID 1773298ノート

反応式

HRID 1773298 の反応式
[Na].[C:2]([O:8]CC)(=O)[CH2:3][C:4]([O-:6])=O.[CH3:11][O:12][C:13]1[CH:14]=[C:15]([CH2:19][CH2:20][NH:21][C:22]([NH2:24])=[O:23])[CH:16]=[CH:17][CH:18]=1>CCO>[CH3:11][O:12][C:13]1[CH:14]=[C:15]([CH2:19][CH2:20][N:21]2[C:2](=[O:8])[CH2:3][C:4](=[O:6])[NH:24][C:22]2=[O:23])[CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 3052719Urea, (3-methoxyphenethyl)-HCID 3595298Propanedioic acid, monoethyl esterHCID 5360545Sodium

生成物 1

HCID 575910951-[2-(3-Methoxyphenyl)ethyl]pyrimidine-2,4,6(1H,3H,5H)-trione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Sodium (236 mg, 10.2 mmol, 2 eq.) was added to degassed EtOH (18 mL), when sodium dissolved completely, ethyl malonate (1.56 mL, 10.2 mmol, 2 eq.) was added and the reaction was refluxed for 1 h. Intermediate 1 (995 mg, 5.12 mmol, 1 eq.) in EtOH (4 mL) was then added and the reaction was refluxed for 1 day. The desired intermediate 37 1-[2-(3-methoxy-phenyl)-ethyl]-pyrimidine-2,4,6-trione precipitated upon addition of 2N aqueous HCl, it was filtered and washed with H2O and finally dried.

後処理

  1. customto degassed EtOH (18 mL), when sodium
  2. dissolutiondissolved completely
  3. temperaturethe reaction was refluxed for 1 h
  4. temperaturethe reaction was refluxed for 1 day
  5. customThe desired intermediate 37 1-[2-(3-methoxy-phenyl)-ethyl]-pyrimidine-2,4,6-trione precipitated upon addition of 2N aqueous HCl, it
  6. filtrationwas filtered
  7. washwashed with H2O
  8. customfinally dried

出典と根拠

ORDレコード
ord-dc0df237194c468a97258c5f293bcd2a
出典データセット
uspto-grants-2016_02
特許番号
US09255095B2

反応ノート

読み込み中…