Sodium Bicarbonate → HCID 131730676, compound

Participants

Reaction Steps

Under an argon atmosphere, the compound (315 mg) obtained in Example 32(7) was dissolved in dimethylformamide (3 mL), and then 28% ammonia water (199 μL) and HATU (2-(1H-azabenzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate methaneaminium) (337 mg) were added, followed by stirring at room temperature for 15 hours. After completion of the reaction, water (10 mL) and then an aqueous saturated sodium hydrogen carbonate were added, followed by extraction twice with dichloromethane (20 mL). The organic layers were combined, washed with saturated brine and then dried over anhydrous magnesium sulfate. After removing anhydrous magnesium sulfate by filtration, the filtrate was concentrated and the resultant residue was purified by silica gel column chromatography (CHROMATOREX NH (trade name), manufactured by Fuji Silysia Chemical Ltd.) (hexane:ethyl acetate=50:50→0:100→ethyl acetate:methanol=100:0→80:20) to obtain the title compound having the following physical properties (yield: 204 mg).

Provenance & Evidence