1,1'-Carbonyldiimidazole → 3,4-Dihydro-3-methyl-2(1H)-quinazolinone
反応式
[C:1]([N:8]1[CH:12]=[CH:11]N=[CH:9]1)([N:3]1[CH:7]=[CH:6]N=C1)=[O:2].CN[CH2:15][C:16]1C=CC=C[C:17]=1N>C1COCC1>[CH3:9][N:8]1[CH2:12][C:11]2[C:7](=[CH:6][CH:15]=[CH:16][CH:17]=2)[NH:3][C:1]1=[O:2]参加物
4
実験手順
1,1'-Carbonyl-diimidazole (16.7 g) is added to a solution of 2-(methylaminomethyl)-aniline (11.2 g) in anhydrous THF (30 ml) under nitrogen. The reaction mixture is refluxed for about 24 hours, stirred for 48 hours at RT and filtered. The filtered precipitate is suspended in 2N HCl for about 40 minutes, filtered, and the filtered solid washed with water and air dried, affording the desired product, M.P. 202-206.5 C., used in the next step without further purification.
後処理
- temperatureThe reaction mixture is refluxed for about 24 hours
- filtrationfiltered
- waitThe filtered precipitate is suspended in 2N HCl for about 40 minutes
- filtrationfiltered
- washthe filtered solid washed with water and air
- customdried
出典と根拠
- ORDレコード
- ord-7801264842fd46cda0c37c153771ce57
- 出典データセット
- uspto-grants-1988_11
- 特許番号
- US04785101
反応ノート
読み込み中…