Chloroacetyl chloride → 1H,2H,3H-pyrido(2,3-b)(1,4)oxazin-2-one

In a 20 ml flask equipped with a reflux apparatus, 3-amino-pyridin-2-ol (300 mg, 2.72 mmol) was dissolved in acetonitrile (27 ml). To the reaction solution was added chloroacetyl chloride (0.24 ml, 3.0 mmol) dropwise at room temperature, followed by Potassium carbonate (940 mg, 6.80 mmol). The mixture was heated at 1000 for 15 hours. After completion of the reaction, acetonitrile was evaporated under the reduced pressure. To the residue was added water and then the mixture was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain white solid (113 mg, 28%).

1. temperatureThe mixture was heated at 1000 for 15 hours
2. customwas evaporated under the reduced pressure
3. additionTo the residue was added water
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate (Na2SO4)
6. filtrationfiltered
7. customevaporated under reduced pressure

ORD-Eintrag

ord-9fb48e7fa890440895e0c5afa8bb2689

Quelldatensatz

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08394792B2