반응 #1468479

반응 방정식

3-phenoxypropionaldehyde

methylmagnesium

methylmagnesium iodide

hydrochloric acid

→

4-phenoxy-2-butanol

수율 67.0%

용매

diethyl ether

반응 조건

후처리

1. 1
   기타by Grignard reaction
2. 2
   온도while maintaining a temperature of not more than 20° C
3. 3
   기타the solution was separated into two phases, which phases
4. 4
   기타were then separated from each other
5. 5
   세척The ether layer was washed with an aqueous sodium bicarbonate solution
6. 6
   세척washed with water
7. 7
   건조dried with anhydrous sodium sulfate
8. 8
   기타condensed under reduced pressure

실험 절차

24.9 g of methyl iodide was reacted with 7.26 g of magnesium in 150 ml of anhydrous diethyl ether to obtain methylmagnesium iodide by Grignard reaction. To a solution consisting of 20 g of 3-phenoxypropionaldehyde and 200 ml of anhydrous diethyl ether was added dropwise the methylmagnesium while maintaining a temperature of not more than 20° C. To the reaction solution was added 25 ml of concentrated hydrochloric acid and the solution was separated into two phases, which phases were then separated from each other. The ether layer was washed with an aqueous sodium bicarbonate solution, washed with water, dried with anhydrous sodium sulfate and then condensed under reduced pressure to obtain 15.0 g of 4-phenoxy-2-butanol having a boiling point of 61° C. to 62° C. at 3 mmHg in a yield of 67%.

출처