Tin atom → 7-Phenyl-1H-pyrido[2,3-b][1,4]oxazin-2(3H)-one
반응식
[N+:1]([C:4]1[C:5]([O:16][CH2:17][C:18]([O:20]CC)=O)=[N:6][CH:7]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:9]=1)([O-])=O.[Sn]>Cl>[C:10]1([C:8]2[CH:7]=[N:6][C:5]3[O:16][CH2:17][C:18](=[O:20])[NH:1][C:4]=3[CH:9]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1참가 물질
4
반응 조건
- 온도
- 2.5 °C
실험 절차
In a 500 ml round-bottomed flask was added ethyl 2-(3-nitro-5-phenylpyridin-2-yloxy)acetate (4.6 g, 15.22 mmol) in hydrochloric acid, 37% (40 ml) to give a yellow suspension. The mixture was cooled to 0-5° C. followed by the portion wise addition of tin powder (9.94 g, 84 mmol). The addition proved to be exothermic. Caution should be taken while adding. The mixture was then stirred at room temperature for further 30 minutes until all foaming ceased. The reaction mixture was heated to 80° C. under a nitrogen atmosphere for 3 hours.
후처리
- customto give a yellow suspension
- additionThe addition
- additionwhile adding
- temperatureThe reaction mixture was heated to 80° C. under a nitrogen atmosphere for 3 hours
출처 및 근거
- ORD 기록
- ord-f13cf9e9ce16442abb54db50a4d6fd1e
- 출처 데이터셋
- uspto-grants-2015_12
- 특허 번호
- US09221838B2
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