Ethyl Methacrylate → 3,4-dihydro-3-methyl-Pyrimido[1,2-a]benzimidazol-2(1H)-one

HRID 215694

반응식

HRID 215694 반응식
[NH2:1][C:2]1[NH:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[C:11](OCC)(=[O:15])[C:12]([CH3:14])=[CH2:13]>COC(C)(C)C>[CH3:13][CH:12]1[CH2:14][N:6]2[C:2](=[N:3][C:4]3[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=32)[NH:1][C:11]1=[O:15]

참가 물질

4

반응물 2

HCID 7343Ethyl MethacrylateHCID 136242-Aminobenzimidazole

생성물 1

HCID 3884553,4-dihydro-3-methyl-Pyrimido[1,2-a]benzimidazol-2(1H)-one

시약·촉매·용매 1

HCID 15413tert-Butyl methyl ether용매

반응 조건

온도
130 °C

실험 절차

5.326 g (40 mmol) 2-aminobenzimidazole and 4.56 g (40 mmol) ethyl methacrylate were dissolved in 25 ml Proglyde DMM. The reactionmixture is heated to 130° C. The reaction is allowed to continue for 7 hours at 130° C. The reactionmixture is allowed to cool down to room temperature and is added to 250 ml tert-butyl methyl ether. The precipitated 3,4-dihydro-3-methyl-pyrimidino[1,2-a]benzimidazol-2(1H)-one was isolated by filtration and recrystallized from 1-methoxy-2-propanol. 2.7 g (33%) of 3,4-dihydro-3-methyl-pyrimidino[1,2-a]benzimidazol-2(1H)-one was isolated (m.p. >260° C.).

후처리

  1. temperatureto cool down to room temperature

출처 및 근거

ORD 기록
ord-2e2cf69afac3486a8889f1bfba064846
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08192918B2

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