Phosphorus oxychloride → HCID 22011950, 화합물
반응식
[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]=1참가 물질
3
실험 절차
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.
후처리
- concentration1 hour at 50° C., the mixture was concentrated in vacuo
- customazeotroping with toluene
- washwashed with sodium bicarbonate solution
- customdried
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-d14b1f41fcf24143a5ffbb6948eb0928
- 출처 데이터셋
- uspto-grants-2004_04
- 특허 번호
- US06723726B1
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