Hydrogen chloride-ethyl acetate → 3-(2,5-dimethyl-1H-pyrrol-1-yl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepine hydrochloride

Temperatur

50 °C

To a solution of 8-benzyl-3-(2,5-dimethyl-1H-pyrrol-1-yl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepine (60 mg) in methanol (4 mL) was added 20% Pd(OH)2/C (10 mg), and the mixture was stirred under a hydrogen atmosphere at 50° C. for 2 hr. The reaction mixture was filtered, and the filtrate was concentrated. To a solution of the obtained crude product in ethyl acetate (4 mL) was added a 4 N hydrogen chloride-ethyl acetate solution (50 μL), and the mixture was stirred for 30 min. The reaction mixture was filtered to give the title compound (28 mg, 56%) as a brown powder.

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate was concentrated
3. customTo a solution of the obtained crude product in ethyl acetate (4 mL)
4. stirringthe mixture was stirred for 30 min
5. filtrationThe reaction mixture was filtered

ORD-Eintrag

ord-5213ace6238c477f80aee23f0940cb38

Quelldatensatz

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08314088B2