反应详情

2.0 g of 2,3-difluoro-4-dodecyloxybenzoic acid, 1.8 g of 4-[(E)-3-(trans-4-pentylcyclohexyl)allyloxy]phenol and 0.1 g of 4-(dimethylamino)pyridine were dissolved in 50 ml of dichloromethane and the solution was treated portionwise within 10 minutes while stirring with 1.4 g of N,N'-dicyclohexylcarbodiimide. The mixture was stirred at room temperature overnight and then filtered. The filtrate was diluted with dichloromethane, washed twice with 50 ml of saturated sodium carbonate solution each time and then with water, dried over magnesium sulphate and concentrated. The crude product obtained was purified by chromatography on silica gel with toluene. The 2,3-difluoro-4-dodecyloxybenzoic acid 4-[(E)-3-(trans-4-pentylcyclohexyl)allyloxy]phenyl ester obtained was recrystallized from ethanol; m.p. (C-SC) 73° C., SC -N 124° C., cl.p. (N-I) 137° C..

1. additionthe solution was treated portionwise within 10 minutes
2. filtrationfiltered
3. additionThe filtrate was diluted with dichloromethane
4. washwashed twice with 50 ml of saturated sodium carbonate solution each time
5. dry with materialwith water, dried over magnesium sulphate
6. concentrationconcentrated
7. customThe crude product obtained
8. customwas purified by chromatography on silica gel with toluene