Methane → HCID 70473491, compound

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Reaction Steps

The product ethyl 8-acetamidomethyl-6,7-dihydro-5-methyl-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylate (1.0 g) from Example 6 was mixed with 25 ml of 6 N hydrochloric acid, and the mixture was heated at reflux for two hours. The mixture was evaporated to dryness, and the residue was triturated with isopropyl alcohol. The solid obtained was dissolved in 20 ml of water. One gram of sodium acetate was added, and the mixture was treated with decolorizing charcoal and filtered. The volume of the solution was reduced to 5 ml, and 5 ml of isopropyl alcohol was added. Seeding was used to provide white crystals of 8-aminomethyl-6,7-dihydro-5-methyl-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid hydrate, m.p. 228°-250° C. (dec.). Analysis: Calculated for C15H16N2O3.1/2H2O: %C, 64.0; %H, 6.1; %N, 10.0; Found: %C, 63.9, %H, 5.9; %N, 9.7. The structural assignment was confirmed by infrared and nuclear magnetic resonance spectral analyses.

Provenance & Evidence