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Water → HCID 13577833, 화합물

HRID 986741
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HRID 986741 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[NH:9][C:8](=[O:15])[NH:7][C:6]2=[O:16].[H-].[Na+].[CH3:19][O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[N:27]1[CH2:32][CH2:31][N:30]([CH2:33][CH2:34]Cl)[CH2:29][CH2:28]1.O>CN(C)C=O>[CH3:19][O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[N:27]1[CH2:28][CH2:29][N:30]([CH2:33][CH2:34][N:7]2[C:6](=[O:16])[C:5]3[C:10](=[CH:11][C:12]([O:13][CH3:14])=[C:3]([O:2][CH3:1])[CH:4]=3)[NH:9][C:8]2=[O:15])[CH2:31][CH2:32]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 1200816,7-Dimethoxy-2,4(1H,3H)-quinazolinedioneHCID 5956731-(2-Chloroethyl)-4-(2-methoxyphenyl)piperazine

생성물 1

HCID 13577833HCID 13577833, 화합물수율 35.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

Two grams of 6,7-dimethoxy-1,2,3,4-tetrahydroquinazoline-2,4-dione was dissolved in 30 ml of dimethylformamide. After adding 1230 mg of sodium hydride thereto under cooling, the mixture was stirred for 10 minutes. Then, 23 grams of 2-[4-(2-methoxyphenyl)-1-piperazinyl]ethyl chloride was added and the stirring was continued at 70° C. for 6 hours. After the reaction was finished, water was added to the reaction mixture and the mixture was extracted with chloroform and concentrated. The resultant residue was purified through the silica gel chromatography and crystallized from methanol to obtain 1.4 g of the titled compound (yield: 35%).

후처리

  1. temperatureunder cooling
  2. waitthe stirring was continued at 70° C. for 6 hours
  3. extractionthe mixture was extracted with chloroform
  4. concentrationconcentrated
  5. customThe resultant residue was purified through the silica gel chromatography
  6. customcrystallized from methanol

출처 및 근거

ORD 기록
ord-28e761f4b4ec402d864a0c6ab7d8b596
출처 데이터셋
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04716161

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