تفاعل #2328979

معادلة التفاعل

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

المردود 68.9%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with toluene
2. 2
   غسيلwashed in turn with water, 10% hydrochloric acid, water, and saturated saline
3. 3
   تجفيفdried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
5. 5
   أخرىthe residue was purified in turn
6. 6
   أخرىby subjecting to column chromatography (silica gel/toluene), recrystallization (methanol/acetone), column chromatography (alumina/acetone)
7. 7
   غسيلwashing with ion-exchange water, silica treatment, and recrystallization (methanol/acetone)

الإجراء التجريبي

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.

المصدر