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

HRID 1773298노트

반응식

HRID 1773298 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dc0df237194c468a97258c5f293bcd2a
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09255095B2

반응 노트

불러오는 중…