반응 #1719481

ord-aaf6df2bc6444097bd83a4eba46fcdcf

반응 방정식

O=CCCOc1ccccc1
3-phenoxypropionaldehyde
[CH3][Mg][I]
methylmagnesium
[CH3][Mg][I]
methylmagnesium iodide
Cl
hydrochloric acid
CC(O)CCOc1ccccc1
4-phenoxy-2-butanol
수율 67.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타by Grignard reaction
  2. 2
    온도while maintaining a temperature of not more than 20° C
  3. 3
    기타separated
  4. 4
    세척The ether layer was washed with an aqueous sodium bicarbonate solution
  5. 5
    세척washed with water
  6. 6
    건조dried with anhydrous sodium sulfate
  7. 7
    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. The reaction solution was added with 25 ml of concentrated hydrochloric acid and separated. 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

DOI: 10.6084/m9.figshare.5104873.v1특허: US04474964uspto-grants-1984_10