Sodium Bicarbonate → HCID 70667981, Verbindung

A solution of the compound prepared in Example 7 (2.00 g), tert-butyl piperidin-4-ylmethylcarbamate (2.72 g) and acetic acid (0.66 mL) in acetonitrile (60 mL) was stirred at room temperature for 30 minutes. Tetramethylammonium triacetoxyborohydride (9.12 g) was added and the reaction was stirred overnight. The reaction was then poured into a saturated aqueous sodium bicarbonate solution and the resulting mixture was extracted three times with ethyl acetate. The combined organics were dried with anhydrous magnesium sulfate and concentrated to a white solid. The solid was triturated with hexane to obtain the title compound (3.90 g) having the following physical data.

1. extractionthe resulting mixture was extracted three times with ethyl acetate
2. dry with materialThe combined organics were dried with anhydrous magnesium sulfate
3. concentrationconcentrated to a white solid
4. customThe solid was triturated with hexane

ORD-Eintrag

ord-c483293dcd164048becde7f92d66eaf8

Quelldatensatz

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08809538B2