反应详情

温度

70 °C

A mixture of 0.1 g of sodium hydride and 25 ml of tetrahydrofuran was treated with 0.5 g of trans-4-propylcyclohexanol while gassing with nitrogen, stirred for a further 2 hours, then treated with 1.0 g of (E)-3-(trans-4-pentylcyclohexyl)allyl bromide and subsequently heated to 70° C. overnight. Thereafter, the reaction mixture was treated with 500 ml of water and extracted four times with 50 ml of hexane each time. The combined organic phases were washed twice with 500 ml of water each time, dried over magnesium sulphate, filtered and then concentrated. The residue was purified by chromatography on silica gel with toluene. The trans-4-propylcyclohexyl (E)-3-(trans-4-pentylcyclohexyl)allyl ether obtained was recrystallized from acetone at -25° C.. This gave 1.2 g of pure product with m.p. (C-I) 26° C..

1. extractionextracted four times with 50 ml of hexane each time
2. washThe combined organic phases were washed twice with 500 ml of water each time
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by chromatography on silica gel with toluene