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

HRID 483234

反応式

HRID 483234 の反応式
Cl[CH2:2][CH2:3][N:4]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][C:5]1=[O:15].[CH3:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1.[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[CH3:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[N:24]1[CH2:29][CH2:28][N:27]([CH2:2][CH2:3][N:4]2[C:13](=[O:14])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[NH:6][C:5]2=[O:15])[CH2:26][CH2:25]1

参加物

7

反応物 4

HCID 13461-(2-Methoxyphenyl)piperazineHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 787663-(2-chloroethyl)(1H,3H)quinazoline-2,4-dione

生成物 1

HCID 1220653-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-2,4(1H,3H)-quinazolinedione収率 86.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 3-(2-chloroethyl)-2,4-(1H,3H)-quinazolinedione (1.57 kg), 1-(2-methoxyphenyl)piperazine (1.34 kg), sodium iodide (1.05 kg) and potassium carbonate (0.49 kg) was dissolved in dimethylformamide (7,000 ml) and the solution was heated at an internal temperature of 80°-85° C. for 7 hours. After completion of the reaction, the mixture was cooled by the addition of water (25 l) and ice (5 kg). The cooled mixture was left for 24 hours and the resulting crystal was collected, washed with water and dried with heat to give 3-[2-[4-(2-methoxyphenyl)-1-piperazinyl]ethyl]-2,4-(1H,3H)quinazolinedione (2.3 kg). Its physicochemical data was the same as that of the products obtained in Example 1.

後処理

  1. temperaturethe solution was heated at an internal temperature of 80°-85° C. for 7 hours
  2. customAfter completion of the reaction
  3. customthe resulting crystal was collected
  4. washwashed with water
  5. customdried
  6. temperaturewith heat

出典と根拠

ORDレコード
ord-637f216f30e04903a3331fe0088869b7
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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