5-Methylcyclohexane-1,3-dione → HCID 67041612, compound

Participants

Reaction Steps

250 mg (1.1 mmol) of 4-chloro-3-(methylamino)-2-nitrobenzoic acid, 410.3 mg (3.3 mmol) of 5-methylcyclohexane-1,3-dione, 275.7 mg (1.4 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride and 13.5 mg (0.1 mmol) of 4-(dimethylamino)pyridine were dissolved in 6 ml of methylene dichloride and stirred at RT for 8 h. This was followed by washing with water and saturated NaHCO3 solution, after which the organic phase was dried over MgSO4 and then the whole was filtered through a small glass frit filled with 1 cm of silica gel, with suction, and the filter product was washed with heptane/ethyl acetate 1:2. The filtrate was concentrated.

Provenance & Evidence