1-benzyl-3-(3-chloropropyl)-5-methyl-2,4(1H,3H)-pyrimidinedione → 3-(3-chloropropyl)-5-methyl-2,4(1H,3H)-pyrimidinedione
反応式
C([N:8]1[CH:13]=[C:12]([CH3:14])[C:11](=[O:15])[N:10]([CH2:16][CH2:17][CH2:18][Cl:19])[C:9]1=[O:20])C1C=CC=CC=1>[Pd].C([O-])=O.[NH4+].CO>[Cl:19][CH2:18][CH2:17][CH2:16][N:10]1[C:11](=[O:15])[C:12]([CH3:14])=[CH:13][NH:8][C:9]1=[O:20]参加物
4
反応条件
- 温度
- 25 °C
実験手順
A mixture of 1-benzyl-3-(3-chloropropyl)-5-methyl-2,4(1H,3H)-pyrimidinedione (1 g, 3.41 mmol), prepared as in Example 19, 10% palladium on carbon (1 g) and 0.1M ammonium formate/methanol (340 mL) was heated 3 hours at reflux under argon. The reaction mixture was allowed to cool to 25° C., then filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with hexane-ethyl acetate (1:1) to give 3-(3-chloropropyl)-5-methyl-2,4(1H,3H)-pyrimidinedione (0.52 g, 2.57 mmol), m.p. 117°-121° C.