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-1320220977a74333a6bd3d1d3e1b4306

Source dataset

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09115139B2