Hydrazine hydrate (1:1) → HCID 76568135, Verbindung

The reaction mixture of racemic (2′R,3R,4′S)-6-chloro-4′-(5-chloro-2-nitro-phenyl)-2′-isopropenylspiro[3H-indole-3,3′-piperidine]-2,6′(1H)-dione (290 mg, 0.65 mmol), Raney Ni (39 mg) and NH2NH2.H2O (320 mg) in methanol was stirred at 80° C. for 0.5 h. The mixture was cooled to 4° C., and concentrated. To the residue were added ethyl acetate (10 mL) and water (10 mL). The organic layer was separated, washed with brine, dried over MgSO4 and concentrated. The residue was purified by column chromatography to give the title compound as a solid (Yield: 260 mg).

1. temperatureThe mixture was cooled to 4° C.
2. concentrationconcentrated
3. additionTo the residue were added ethyl acetate (10 mL) and water (10 mL)
4. customThe organic layer was separated
5. washwashed with brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customThe residue was purified by column chromatography

ORD-Eintrag

ord-6e422cb4566f4f5f9a8b60d7325f69d6

Quelldatensatz

uspto-grants-2009_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07495007B2