تفاعل #2025289

معادلة التفاعل

hydrochloric acid

acetic acid anhydride

(+)-3-phenyl-1-butanol

toluene

→

(+)-1-acetoxy-3-phenylbutane

المردود 99.0%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   أخرىInto a four-necked flask provided with a stirring means
2. 2
   أخرىThe mixture was reacted for 4 hours while temperature
3. 3
   درجة الحرارةbeing maintained at 40°-50° C
4. 4
   أخرىAfter completion of the reaction
5. 5
   استخلاصextracted
6. 6
   غسيلThe resulting organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate aqueous solution ad water in the order
7. 7
   تركيزThe thus-obtained organic layer was concentrated under a reduced pressure

الإجراء التجريبي

Into a four-necked flask provided with a stirring means and a thermometer, 150 g (1 mol) of (+)-3-phenyl-1-butanol (XXVI-60), 500 ml of toluene and 200 ml of pyridine were charged, and 122.4 g (1.2 mol) of acetic acid anhydride and 1 g of 4-dimethylaminopyridine were further added thereto. The mixture was reacted for 4 hours while temperature being maintained at 40°-50° C. After completion of the reaction, the reaction mixture was poured into 500 ml of 4N hydrochloric acid, extracted and fractionated. The resulting organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate aqueous solution ad water in the order. The thus-obtained organic layer was concentrated under a reduced pressure to obtain 190 g of (+)-1-acetoxy-3-phenylbutane (XXV-60) with yield of 99.0%.

المصدر