Water → 3-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-2,4(1H,3H)-quinazolinedione

HRID 483233

반응식

HRID 483233 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][NH:17][C:18](=[O:26])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[NH2:25])[CH2:11][CH2:10]1.N[C:28](N)=[O:29].O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][N:17]2[C:18](=[O:26])[C:19]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[NH:25][C:28]2=[O:29])[CH2:11][CH2:10]1

참가 물질

5

반응물 3

HCID 962WaterHCID 1176UreaHCID 132291672-Amino-N-{2-[4-(2-methoxyphenyl)piperazin-1-yl]ethyl}benzamide

생성물 1

HCID 1220653-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-2,4(1H,3H)-quinazolinedione수율 92.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-(2-Methoxyphenyl)-4-[2-(2-aminobenzoyl)aminoethyl]piperazine (3.54 g) and urea (1.2 g) were dissolved in dimethylformamide (20 ml) and the resulting solution was heated at an external temperature of 140° to 180° C. for 5 to 8 hours. After completion of the reaction, water (200 ml) was added to the reaction mixture and the resulting crystal was filtered off. Upon recrystallization from dioxane, 3-[2-[4-(2-methoxyphenyl)-1-piperazinyl]ethyl]2,4-(1H,3H)-quinazolinedione (3.5 g) was obtained as needles. Its physicochemical data was the same as that of the product obtained in (a).

후처리

  1. temperaturethe resulting solution was heated at an external temperature of 140° to 180° C. for 5 to 8 hours
  2. additionwas added to the reaction mixture
  3. filtrationthe resulting crystal was filtered off
  4. customUpon recrystallization from dioxane

출처 및 근거

ORD 기록
ord-fa6f930c11a843969a837ae56f8048bd
출처 데이터셋
uspto-grants-1986_03
특허 번호
US04578465

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