反应 #2328979

反应方程式

water

trans-4-(trans-4-vinylcyclohexyl)cyclohexylmethyl methanesulfonate

2,3-difluoro-4-ethoxyphenol

tripotassium phosphate

→

4-ethoxy-2,3-difluoro-1-(trans-4-(trans-4-vinylcyclohexyl)cyclohexyl)methoxybenzene

收率 68.9%

溶剂

DMF

反应条件

后处理

1. 1
   萃取extracted with toluene
2. 2
   洗涤washed in turn with water, 10% hydrochloric acid, water, and saturated saline
3. 3
   干燥dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
5. 5
   其他the residue was purified in turn
6. 6
   其他by subjecting to column chromatography (silica gel/toluene), recrystallization (methanol/acetone), column chromatography (alumina/acetone)
7. 7
   洗涤washing with ion-exchange water, silica treatment, and recrystallization (methanol/acetone)

实验过程

9.8 g of trans-4-(trans-4-vinylcyclohexyl)cyclohexylmethyl methanesulfonate and 5.96 g of 2,3-difluoro-4-ethoxyphenol were dissolved in 90 mL of DMF. 10.4 g of tripotassium phosphate was added, followed by stirring at 90 to 100° C. for 3 hours. The reaction mixture was poured into water, extracted with toluene, washed in turn with water, 10% hydrochloric acid, water, and saturated saline and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified in turn by subjecting to column chromatography (silica gel/toluene), recrystallization (methanol/acetone), column chromatography (alumina/acetone), washing with ion-exchange water, silica treatment, and recrystallization (methanol/acetone) to obtain 8.5 g of 4-ethoxy-2,3-difluoro-1-(trans-4-(trans-4-vinylcyclohexyl)cyclohexyl)methoxybenzene (IIIa) as a colorless crystal.

来源