Isobutylamine → HCID 18324831, compound

Participants

Reaction Steps

A mixture of isobutylamine (27.2 mL) and the hydrobromide salt of Example 8, Step B (9.4 g) was heated at 90° C. under nitrogen for 1 hour. The reaction was cooled and partitioned between dichloromethane and 1N sodium hydroxide. The aqueous layer was extracted with dichloromethane, and the combined extracts were dried over sodium sulfate and concentrated in vacuo to give a brown oil. The crude material was dissolved in dichloromethane and absorbed onto a column of Merck-60 flash silica gel. Elution with 25% ethyl acetate in hexane followed by 80:20 dichloromethane-methanol containing 0.2% ammonium hydroxide gave the title compound (6.0 g, 85.9%) as a brown oil, which was used as such in the next step.

Provenance & Evidence