Water → Pyrazolo(4,3-e)pyrido(3,2-b)(1,4)diazepin-10(1H)-one, 4,9-dihydro-1,3,9-trimethyl-
反応式
[CH3:1][N:2]1[C:11]2[C:10](=[O:12])[NH:9][C:8]3[CH:13]=[CH:14][CH:15]=[N:16][C:7]=3[NH:6][C:5]=2[C:4]([CH3:17])=[N:3]1.[H-].[Na+].[CH3:20]I.O>CN(C)C=O>[CH3:1][N:2]1[C:11]2[C:10](=[O:12])[N:9]([CH3:20])[C:8]3[CH:13]=[CH:14][CH:15]=[N:16][C:7]=3[NH:6][C:5]=2[C:4]([CH3:17])=[N:3]1参加物
6
反応条件
- 温度
- 60 °C
実験手順
An amount of 5.25 gm (0.025 mol) of 1,3-dimethyl-1,4,9,10-tetrahydro-pyrazolo[4,3-e]pyrido[3,2-b][1,4]diazepin-10-one was dissolved in 25 ml of N,N-dimethylformamide and mixed with 1.2 gm of a 55% sodium hydride dispersion in mineral oil. After stirring for 2 hours at 60° C., the solution was cooled to 40° C., and 2.2 ml of methyl iodide were added dropwise. Subsequently the mixture was stirred for 3 hours at 40° C., and after addition of 50 ml of water and cooling in the ice-bath, the desired compound was obtained in crystals. The crystals were recovered by suction filtration, and the mineral oil was washed out by means of petroleum ether.
後処理
- temperaturethe solution was cooled to 40° C.
- stirringSubsequently the mixture was stirred for 3 hours at 40° C.
出典と根拠
- ORDレコード
- ord-48ec64fca1f34e6c9d3739b1b6b48e44
- 出典データセット
- uspto-grants-1983_04
- 特許番号
- US04381303
反応ノート
読み込み中…