2-[2-(9H-carbazol-1-ylamino)phenyl]propan-2-ol → 7,7-dimethyl-12,13-dihydro-7H-indolo[3,2-c]acridine
反応式
[C:1]1([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21](O)([CH3:23])[CH3:22])[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1>O>[CH3:22][C:21]1([CH3:23])[C:2]2[CH:3]=[CH:4][C:5]3[C:6]4[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=4[NH:12][C:13]=3[C:1]=2[NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]1=2参加物
3
反応条件
- 温度
- 0 °C
実験手順
63 g (200 mmol) of 2-[2-(9H-carbazol-1-ylamino)phenyl]propan-2-ol are initially introduced in 268 g (2734 mmol) of polyphosphoric acid under protective gas and cooled to 0° C. The mixture is subsequently stirred at 100° C. for 3 h and then cooled to room temperature. Water is added to the mixture with ice cooling, the mixture is extracted with ethyl acetate, and the solvent is removed in vacuo. The content of product according to 1H-NMR is about 96% with an overall yield of 53 g (90%).
後処理
- temperaturecooled to room temperature
- extractionthe mixture is extracted with ethyl acetate
- customthe solvent is removed in vacuo
出典と根拠
- ORDレコード
- ord-6cee9cc7d498451f963df8108bf9e05c
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835626B2
反応ノート
読み込み中…