反応 #2025285

反応方程式

hydrochloric acid

acetic acid

4-phenyl-2-butanol

toluene

→

2-acetoxy-4-phenylbutane

収率 98.5%

溶媒

pyridine

反応条件

後処理

1. 1
   workup.ADDITIONwere charged
2. 2
   その他to react them for 4 hours
3. 3
   温度while temperature being maintained at 40°-50° C
4. 4
   その他After completion of the reaction
5. 5
   抽出extracted
6. 6
   洗浄an organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate solution and water in the order
7. 7
   濃縮The thus-obtained organic layer was concentrated under a reduced pressure

実験手順

Into a four-necked flask provided with a thermometer and a stirrer, 150 g (1 mol) of 4-phenyl-2-butanol (XXX-35), 500 ml of toluene and 200 ml of pyridine were charged. 122.4 g (1.2 mol) of anhydrous acetic acid and 1 g of 4-dimethylaminopyridine were further added thereto to react them 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 solution, extracted and fractionated, and then an organic layer was washed with 1N hydrochloric acid, water, 5% sodium bicarbonate solution and water in the order. The thus-obtained organic layer was concentrated under a reduced pressure to obtain 189 g of 2-acetoxy-4-phenylbutane (XXIX-35) with yield of 98.5%.

出典