3-Methylbutanal → HCID 59487403, compound

Participants

Reaction Steps

500 mg (5.81 mmol) of methyl 3-oxopentanoate, 755 mg (5.81 mmol) of 2,2-dimethyl-1,3-dioxane-4,6-dione and 492 mg (6.39 mmol) of ammonium acetate were initially charged in 5 ml of acetic acid, and 0.623 ml (5.81 mmol) of 3-methylbutyraldehyde was added. The mixture was then stirred for 14 h each at room temperature and at 130° C. After removal of the volatile components on a rotary evaporator, the residue was purified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% formic acid, gradient 20:80→95:5). Drying under high vacuum gave 390 mg (28% of theory) of the target compound.

Provenance & Evidence