Formic Acid → 1H-Purine-2,6-dione, 3,7-dihydro-3-cyclopropyl-
反応式
[CH:1]1([N:4]2[C:9]([NH2:10])=[C:8]([NH2:11])[C:7](=[O:12])[NH:6][C:5]2=[O:13])[CH2:3][CH2:2]1.[CH:14](O)=O>>[CH:1]1([N:4]2[C:9]3[N:10]=[CH:14][NH:11][C:8]=3[C:7](=[O:12])[NH:6][C:5]2=[O:13])[CH2:3][CH2:2]1参加物
3
実験手順
A solution of 12 g of 1-cyclopropyl-5,6-diamino-2,4-(1H,3H)-pyrimidinedione (IV) in 50 ml of formic acid was refluxed for 2 hours. The hot solution was filtered and 30 ml of chloroform was added and ether was then added slowly. The received crystals were filtered off. Yield 11.2 g (V). The amide (V) was refluxed in 40 ml of 2N NaOH for 1 hour and then neutralized with 5N HCl. The crystals were filtered off. Yield 7 g (60%) (VI) NMR (see Table I).
後処理
- filtrationThe hot solution was filtered
- addition30 ml of chloroform was added
- additionether was then added slowly
- filtrationThe received crystals were filtered off
- temperatureThe amide (V) was refluxed in 40 ml of 2N NaOH for 1 hour
- filtrationThe crystals were filtered off
出典と根拠
- ORDレコード
- ord-4af039f1ef5641d799e9a93d12bc2042
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04644001
反応ノート
読み込み中…