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

HRID 483233

反応式

HRID 483233 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fa6f930c11a843969a837ae56f8048bd
出典データセット
uspto-grants-1986_03
特許番号
US04578465

関連ノート

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