Phosphorus oxychloride → 3-Amino-5-morpholinopicolinonitrile
반응식
[NH2:1][C:2]1[C:3]([C:14]([NH2:16])=O)=[N:4][CH:5]=[C:6]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:7]=1.P(Cl)(Cl)(Cl)=O>C(#N)C>[NH2:1][C:2]1[C:3]([C:14]#[N:16])=[N:4][CH:5]=[C:6]([N:8]2[CH2:9][CH2:10][O:11][CH2:12][CH2:13]2)[CH:7]=1참가 물질
4
실험 절차
A stirred solution of 3-amino-5-morpholinopicolinamide (0.35 g, 1.57 mmol) in acetonitrile (10 mL) was treated with phosphorus oxychloride (0.29 mL, 3.15 mmol). The reaction was heated at reflux for 1 h. After this time the reaction was cooled to rt and evaporated in vacuo. The residue was dissolved in Et2O (10 mL) and treated with 4.0M HCl in dioxane (0.2 mL). The resulting solid was filtered and dried under vacuum to give 3-amino-5-morpholinopicolinonitrile. Mass Spectrum (ESI) m/e=205.2 (M+1).
후처리
- temperatureThe reaction was heated
- temperatureat reflux for 1 h
- customevaporated in vacuo
- dissolutionThe residue was dissolved in Et2O (10 mL)
- additiontreated with 4.0M HCl in dioxane (0.2 mL)
- filtrationThe resulting solid was filtered
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-f3d7308b25604fb2848e703a88694e44
- 출처 데이터셋
- uspto-grants-2015_01
- 특허 번호
- US08940724B2
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