Methanol → HCID 68775975, compound

Participants

Reaction Steps

To a solution of 9-fluoro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester, (1.45 g, 4.76 mmol) in dry DCM (15 mL) was added trifluoroacetic acid (14.30 mL, 3 mL/mmol) at 0° C. The reaction mixture was stirred at r.t. for 2 h under argon. After completion of the reaction as confirmed by TLC, MeOH (2×10 mL) was added and the reaction mixture was evaporated under vacuo to remove excess of solvent and trifluoroacetic acid. The remaining solvents were removed under vacuo and 9-fluoro-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene trifluoroacetate (1.50 g, 4.71 mmol, 99%) was obtained as thick brown jelly. The crude compound was used as such without any further purification for the next step.

Provenance & Evidence