Water → HCID 839770、化合物
反応式
Cl[C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1.O>O1CCCC1>[N:13]1([C:2]2[N:11]=[C:10]([N:13]3[CH2:17][CH2:16][CH2:15][CH2:14]3)[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)[CH2:17][CH2:16][CH2:15][CH2:14]1参加物
5
実験手順
Ten grams of 2,4-dichloroquinazoline was added carefully to a solution of 25 ml of pyrrolidine in 200 ml of tetrahydrofuran. The resulting mixture was heated at reflux overnight and then was poured into a mixture of ice and water. The resulting mixture was extracted several times with ether. The ether extracts were combined and washed with water. The ether phase then was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was recrystallized from a 1:1 benzene:hexane mixture to give 10.1 g of 2,4-bispyrrolidinylquinazoline; m.p. 127°-129°. The following analytical data were obtained:
後処理
- temperatureThe resulting mixture was heated
- temperatureat reflux overnight
- extractionThe resulting mixture was extracted several times with ether
- washwashed with water
- dry with materialThe ether phase then was dried over anhydrous sodium sulfate
- customThe solvent was removed by distillation
- customthe residue was recrystallized from a 1:1 benzene
出典と根拠
- ORDレコード
- ord-76218f30963c4296bd637a5045e948a6
- 出典データセット
- uspto-grants-1977_09
- 特許番号
- US04048312
反応ノート
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