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Water → HCID 13577833、化合物

HRID 986741
ノート
印刷プレビュー

反応式

HRID 986741 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 13577833HCID 13577833、化合物収率 35.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-28e761f4b4ec402d864a0c6ab7d8b596
出典データセット
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04716161

反応ノート

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