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

HRID 483234

반응식

HRID 483234 반응식
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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-637f216f30e04903a3331fe0088869b7
출처 데이터셋
uspto-grants-1986_03
특허 번호
US04578465

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