Phosphorus oxychloride → HCID 22011950、化合物
反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[N:17]=[CH:16][C:10]3[N:11]=[CH:12][NH:13][C:14](=O)[C:9]=3[CH:8]=2)=[N:4][N:3]=1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:14]1[C:9]2[CH:8]=[C:7]([C:5]3[O:6][C:2]([CH3:1])=[N:3][N:4]=3)[N:17]=[CH:16][C:10]=2[N:11]=[CH:12][N:13]=1参加物
3
実験手順
6-(5-Methyl-1,3,4-oxadiazol-2-yl)-pyrido[3,4-d]pyrimidin-4-one (0.5 g) was treated with phosphorus oxychloride at room temperature under N2. After 1 hour at room temperature and 1 hour at 50° C., the mixture was concentrated in vacuo, azeotroping with toluene, then taken up in ethyl acetate, washed with sodium bicarbonate solution, dried and concentrated in vacuo to give the title compound (0.17 g) as an orange solid; δH CDCl3 9.68 (1H,s), 9.30 (1H,s), 8.96 (1H,s), 2.75 (3H,s); m/z (M+1+) 248.
後処理
- concentration1 hour at 50° C., the mixture was concentrated in vacuo
- customazeotroping with toluene
- washwashed with sodium bicarbonate solution
- customdried
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-d14b1f41fcf24143a5ffbb6948eb0928
- 出典データセット
- uspto-grants-2004_04
- 特許番号
- US06723726B1
反応ノート
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