Formic Acid → 4-Ethenylcyclohexanone

103.3 g of the compound (22), 86.5 g of 98% formic acid and 200 mL of toluene were added to a reactor under nitrogen atmosphere, and stirred under refluxing and heating for 2 hours. After confirming that the reaction had been completed by GC analysis, the reaction mixture was poured into and mixed with 500 mL of brine at 0° C. The mixture was separated into an organic layer and an aqueous layer by standing still, so as to attain extraction to the organic layer. The resulting organic layer was fractionated and washed with brine, followed by drying over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The resulting residue was distilled under reduced pressure to obtain 66.7 g of 4-vinylcyclohexanone (23) as a colorless transparent liquid.

1. temperatureunder refluxing
2. temperatureheating for 2 hours
3. additionthe reaction mixture was poured into and
4. customThe mixture was separated into an organic layer
5. extractionextraction to the organic layer
6. washwashed with brine
7. dry with materialby drying over anhydrous magnesium sulfate
8. customthe solvent was removed by distillation under reduced pressure
9. distillationThe resulting residue was distilled under reduced pressure

ORD 기록

ord-1285cec7da1949c397cb77883f2d0f9d

출처 데이터셋

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07695777B2