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

HRID 1784063노트

반응식

HRID 1784063 반응식
[CH3:1][CH2:2][O-:3].[Na+].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH2:13][CH2:14][NH:15][C:16]([NH2:18])=[O:17])[CH:10]=[CH:11][CH:12]=1.Cl.O.C[CH2:22][OH:23]>>[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH2:13][CH2:14][N:15]2[C:2](=[O:3])[CH2:1][C:22](=[O:23])[NH:18][C:16]2=[O:17])[CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 702Ethanol3회HCID 962WaterHCID 2723922Sodium ethoxideHCID 3052719Urea, (3-methoxyphenethyl)-2회

생성물 1

HCID 575910951-[2-(3-Methoxyphenyl)ethyl]pyrimidine-2,4,6(1H,3H,5H)-trione수율 74%

실험 절차

To a solution of NaOEt (144 mmol, fleshly prepared from 3.3 g of Na) in EtOH (80 mL), a solution of ethyl malonate (2) (22 mL, 144 mmol) in EtOH (250 mL) was added. The mixture was refluxed then added a solution of [2-(3-methoxy-phenyl)-ethyl]-urea (2) (23.3 g, 120 mmol) in EtOH (300 mL). The reaction mixture was refluxed overnight, then cooled to room temperature. The mixture was acidified carefully with 1M HCl aq. then poured into water (1 L). The precipitate which was formed was collected by filtration, washed with water then dried under reduced pressure to give the title compound (23.2 g, 74%). MS (ESI) (M+H)+ 263.

후처리

  1. temperatureThe mixture was refluxed
  2. temperatureThe reaction mixture was refluxed overnight
  3. customThe precipitate which was formed
  4. filtrationwas collected by filtration
  5. washwashed with water
  6. customthen dried under reduced pressure

출처 및 근거

ORD 기록
ord-9f43836919cc44168d960ef77667b36f
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07501512B2

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