Ethanol → 3,7-dihydro-8-methyl-3-propyl-1H-purine-2,6-dione
反応式
[NH2:1][C:2]1[C:3](=[O:13])[NH:4][C:5](=[O:12])[N:6]([CH2:9][CH2:10][CH3:11])[C:7]=1[NH2:8].[CH2:14](O)[CH3:15]>C(O)(=O)C>[CH3:14][C:15]1[NH:1][C:2]2[C:3](=[O:13])[NH:4][C:5](=[O:12])[N:6]([CH2:9][CH2:10][CH3:11])[C:7]=2[N:8]=1参加物
4
実験手順
A solution of 22.6 g of 5,6-diamino-1-propyl-2,4-(1H,3H)-pyrimidinedione in 50 ml of acetic acid was refluxed for 2 hours. 30 ml of ethanol was added. The received crystals were filtered off. Yield 19.8 g. The amide was refluxed in 80 ml of 2N NaOH for 2 hours and then neutralized with 5N HCl. The crystals were filtered off and recrystallized from 2.1 l ethanol. Yield 9.8 g (38%) (XXXXVI) NMR (see Table I).
後処理
- filtrationThe received crystals were filtered off
- temperatureThe amide was refluxed in 80 ml of 2N NaOH for 2 hours
- filtrationThe crystals were filtered off
- customrecrystallized from 2.1 l ethanol
出典と根拠
- ORDレコード
- ord-6342188adb714c58b43464f01a451963
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04548818
反応ノート
読み込み中…