Reaktion #10677

Reaktionsgleichung

Intermediate 132

4-[1-(4-methoxybenzyl)amino-5-isoquinolyl]amino-1-(tert-butoxycarbonyl)piperidine

→

title compound

Ausbeute 99.6%

4-(1-amino-5-isoquinolyl)amino-1-(tert-butoxycarbonyl)piperidine

Ausbeute 99.6%

Lösungsmittel

trifluoroacetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvent was evaporated under reduced pressure
2. 2
   workup.ADDITIONThe residue was added with dioxane (3 ml), 2 N aqueous sodium hydroxide (1 ml) and 2 di-t-butyl dicarbonate (393 mg)
3. 3
   SonstigeThe solvent was evaporated under reduced pressure
4. 4
   Sonstigethe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate:isopropylamine=5:5:1)

Vorschrift

A solution of Intermediate 132 (270 mg) in 95% trifluoroacetic acid (5 ml) was stirred at 50° C. for 16 hours, and the solvent was evaporated under reduced pressure. The residue was added with dioxane (3 ml), 2 N aqueous sodium hydroxide (1 ml) and 2 di-t-butyl dicarbonate (393 mg) and stirred at room temperature for 1 hour. The solvent was evaporated under reduced pressure, and then the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate:isopropylamine=5:5:1) to obtain the title compound (199 mg).

Quelle