Morpholine → 6-(Morpholin-4-yl)pyridin-2-amine
反応式
Cl[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=1.[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1>>[N:9]1([C:2]2[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=2)[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1参加物
3
反応条件
- 温度
- 225 °C
実験手順
6-Chloro-2-pyridinamine (1 g, 7.78 mmol) was dissolved in morpholine (6.80 ml, 78 mmol) and heated to 225° C. in a microwave reactor for 60 minutes (˜400 W; 5 mbar). The reaction was cooled to rt and concentrated. The crude product was taken up in DCM (50 mL). After filtration of white solids the crude product was concentrated and purified by silica gel column chromatography eluting with 20-50% EtOAc/hexanes to afford 1 g (5.58 mmol, 72%) of the title compound as a pale yellow solid. LC/MS: (M+H)+: 179.9.
後処理
- temperatureThe reaction was cooled to rt
- concentrationconcentrated
- filtrationAfter filtration of white solids the crude product
- concentrationwas concentrated
- custompurified by silica gel column chromatography
- washeluting with 20-50% EtOAc/hexanes
出典と根拠
- ORDレコード
- ord-6de20908c8c64dcea6bc3a5bb4a85a07
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08901119B2
反応ノート
読み込み中…