반응 #2025289

반응 방정식

hydrochloric acid

acetic acid anhydride

(+)-3-phenyl-1-butanol

toluene

→

(+)-1-acetoxy-3-phenylbutane

수율 99.0%

용매

pyridine

반응 조건

후처리

1. 1
   기타Into a four-necked flask provided with a stirring means
2. 2
   기타The mixture was reacted for 4 hours while temperature
3. 3
   온도being maintained at 40°-50° C
4. 4
   기타After completion of the reaction
5. 5
   추출extracted
6. 6
   세척The resulting organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate aqueous solution ad water in the order
7. 7
   농축The thus-obtained organic layer was concentrated under a reduced pressure

실험 절차

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%.

출처