Trifluoroacetic acid → HCID 22036441, compound

Participants

Reaction Steps

TFA (1.5 mL) was added to a solution of the product from Step 2 (112 mg, 0.22 mmol) in CH2Cl2(1.5 mL) at 0° C. and the mixture was stirred under inert atmosphere for 1 h. The reaction mixture was diluted with CH2Cl2 and washed with 2 M aqueous NaOH (×4) and brine. The organic layer was dried (MgSO4) and concentrated. The crude solid product (83 mg) was purified by column chromatography on silica using CHCl3/MeOH (9:1)+1% NH3 as eluent to give the title compound as an oil that solidified after repeated additions of pentane: yield 67 mg (75%); MS m/z 409 (M+H)+. Anal. (C21H24N6O3.0.6H2O.0.1C5H12) C, H, N.

Provenance & Evidence