Potassium Carbonate → HCID 53792155, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 14 (2.12 g, 8.62 mmol), hydrazine hydrate (55% in water, 7.4 mL, 131 mmol) and potassium carbonate (3.2 g, 23.2 mmol) in diethylene glycol (21 mL) was heated at 150° C. (bath temperature) for 3 hr. After cooled to ambient temperature, the mixture was poured into ice water and extracted with n-hexane. The combined organic layers were washed with cold diluted hydrochloric acid, water, sodium bicarbonate solution and brine, and dried over sodium sulfate. Filtration and concentration gave 1.81 g of an oily material, which was purified by column chromatography (silica gel 20 g, 1-2% ethyl acetate in n-hexane) to give 1.69 g (85.1%) of 15, as a colorless oil.

Provenance & Evidence