反应详情

A solution of 2.1 g of 4-[3-(trans-4-pentylcyclohexyl)-1-propyloxy]benzaldehyde and 1.2 g of 2-pentyl-1,3-propanediol in 50 ml of toluene was treated with 2 drops of 10% (vol., sulfuric acid. The mixture was heated to boiling for 2.5 hours, with the resulting water being distilled off simultaneously. Then, 4 drops of triethylamine were added to the reaction mixture. After cooling the mixture was washed with 20 ml of 1N sodium hydrogen carbonate solution and twice with 20 ml of water each time, dried over sodium sulfate, filtered and concentrated. Chromatography of the residue on silica gel with toluene gave 0.6 g of trans-5-pentyl-2-(4-[3-(trans-4-pentylcyciohexyl)-1-propyloxy]phenyl)-1,3-dioxane. M.p. (C-SB) 65° C. transition SB -N 73° C., cl.p (N-I) 128° C.

1. temperatureThe mixture was heated
2. distillationdistilled off simultaneously
3. additionThen, 4 drops of triethylamine were added to the reaction mixture
4. temperatureAfter cooling the mixture
5. washwas washed with 20 ml of 1N sodium hydrogen carbonate solution and twice with 20 ml of water each time
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated