Hydrochloric Acid → HCID 66993437, compound

To a solution of tert-butyl 3-[ethyl(1-methylethyl)amino]-6,7-dihydropyrazino[2,3-f][1,4]oxazepine-8(9H)-carboxylate (10 mg) in ethyl acetate (0.1 ml) was added 4 N hydrogen chloride-ethyl acetate solution (0.5 ml), and the mixture was stirred for 30 min. The reaction mixture was basified with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The aqueous layer was extracted again with ethyl acetate. The combined organic layer was washed with water and saturated brine, dried over magnesium sulfate, and concentrated. To a solution of the obtained crude product in methanol (0.5 mL) was added 1.0 N hydrochloric acid (33 μL), and the mixture was stirred for 5 min. The reaction mixture was concentrated, and the obtained crystals were purified by recrystallization (ethanol-diisopropyl ether) to give the title compound (10 mg, 100%) as a pale-yellow powder.

1. extractionextracted with ethyl acetate
2. extractionThe aqueous layer was extracted again with ethyl acetate
3. washThe combined organic layer was washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customTo a solution of the obtained crude product in methanol (0.5 mL)
7. stirringthe mixture was stirred for 5 min
8. concentrationThe reaction mixture was concentrated
9. customthe obtained crystals were purified by recrystallization (ethanol-diisopropyl ether)

ORD record

ord-0df3ec674412458789d86f3ea688c996

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08318722B2