تفاعل #1121717

معادلة التفاعل

ammonium chloride

thionyl chloride

4-{[6-(acryloyloxy)hexyl]oxy}benzoic acid

4-(6-bromohexyloxy)phenol

→

4-(6-bromo hexyloxy)phenyl 4-{[6-(acryloyloxy)hexyl]oxy}benzoate

المردود 59.9%

المذيبات

tetrahydrofurane

triethyl amine

ظروف التفاعل

المعالجة

1. 1
   أخرىwas adjusted to a temperature of 0° C. (Celsius)
2. 2
   workup.STIRRINGstirred at 0° C. (Celsius) for 1 hour
3. 3
   workup.STIRRINGstirred at a room temperature overnight
4. 4
   أخرىThe resulting reaction mixture
5. 5
   استخلاصwas extracted three times with ethyl acetate (50 ml (milliliters)), and waster
6. 6
   أخرىwas removed over magnesium sulfate
7. 7
   أخرىThen, the solvents were evaporated
8. 8
   أخرىthe resulting reaction mixture
9. 9
   أخرىwas then purified

الإجراء التجريبي

4-{[6-(acryloyloxy)hexyl]oxy}benzoic acid (4) (2.8 g (grams)) was dissolved in tetrahydrofurane (THF, 100 ml (milliliters)) at a room temperature, and a temperature of the resulting mixture was adjusted to a temperature of 0° C. (Celsius). Then, thionyl chloride (12 ml (milliliters), 1M in THF) was added to the mixture, and stirred for 30 minutes. Then, 4-(6-bromohexyloxy)phenol (2.5 g (grams)) and triethyl amine (13 ml (milliliters)) were added to the resulting reaction mixture, stirred at 0° C. (Celsius) for 1 hour, and then stirred at a room temperature overnight. Next day, a saturated ammonium chloride aqueous solution was poured into the reaction mixture, and the reaction was completed. The resulting reaction mixture was extracted three times with ethyl acetate (50 ml (milliliters)), and waster was removed over magnesium sulfate. Then, the solvents were evaporated, and the resulting reaction mixture was then purified using a column chromatography (developer solution: ethylacetate/hexane=1/2 volume ratio) to obtain 4-(6-bromo hexyloxy)phenyl 4-{[6-(acryloyloxy)hexyl]oxy}benzoate (5) (3 g (grams)).

المصدر