HCID 3991306、化合物 → 3-benzyl-5-methyl-1H-pyrimidine-2,4-dione
反応式
C([N:8]1[CH:13]=[C:12]([CH3:14])[C:11](=[O:15])[N:10]([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]1=[O:23])C1C=CC=CC=1>[Pd].C([O-])=O.[NH4+]>[CH2:16]([N:10]1[C:11](=[O:15])[C:12]([CH3:14])=[CH:13][NH:8][C:9]1=[O:23])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1参加物
4
実験手順
A mixture of 1,3-dibenzyl-5-methyl-2,4(1H,3H)-pyrimidinedione (2 g, 6.5 mmol), 5% palladium on carbon (3 g) and 0.4N ammonium formate (250 mL in methanol) was heated 1.5 hours at reflux. The reaction mixture then was filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with methylene chloride/methanol (95:5) to give 3-benzyl-5-methyl-2,4(1H,3H)-pyrimidinedione, m.p. 208°-210° C.
後処理
- temperaturewas heated 1.5 hours
- temperatureat reflux
- filtrationThe reaction mixture then was filtered
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography on silica gel eluting with methylene chloride/methanol (95:5)
出典と根拠
- ORDレコード
- ord-967537bb05594edb93591d4f289536eb
- 出典データセット
- uspto-grants-1999_01
- 特許番号
- US05859014
反応ノート
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