反应详情

A mixture of 0.5 g of (E)-3-(trans-4-pentylcyclohexyl)allyl alcohol, 0.3 g of 4-methoxyphenol, 0.4 g of diethyl azodicarboxylate, 0.6 g of triphenylphosphine and 25 ml of absolute tetrahydrofuran was stirred at room temperature overnight and then concentrated. The residue was suspended with 50 ml of hot hexane and filtered. The filtrate was concentrated. Chromatography of the residue on silica gel with toluene/hexane (vol. 1:1) and recrystallization from methanol gave pure 4-methoxyphenyl (E)-3-(trans-4-pentylcyclohexyl)allyl ether with m.p. (C-N) 45° C. and cl.p. (N-I) 46° C.

1. concentrationconcentrated
2. filtrationfiltered
3. concentrationThe filtrate was concentrated
4. customChromatography of the residue on silica gel with toluene/hexane (vol. 1:1) and recrystallization from methanol