英语翻译Aryl aldehyde was added to the solution of 85% KOH(1.2 e
英语翻译
Aryl aldehyde was added to the solution of 85% KOH
(1.2 eq) in MeOH (50 mL) and H2O (10 mL) at 0 3C.
After dissolution,aryl methyl ketone (1.0 eq) was added
over a period of 10 min.The mixture was then stirred
for 3 h at 0 3C.A solid product precipitated was filtered,
washed with cold MeOH,and dried to yield 60.3–
97.5%.Utilizing the same procedure,thirty-two compounds
were synthesized.
A mixture of acetyl pyridine,iodine (1.2 eq) and pyridine
60 mL was refluxed for 3 h.The solid product precipitated
was cooled to 0 3C and filtered.The product
was washed with cold pyridine and dried to afford 4–6
in quantitative yield.
A mixture of 3 (R1 = a–h,R2 = a–d),dry ammonium acetate
and 4,5,or 6 in dry MeOH was heated to 80 3C for
12–24 h under nitrogen gas.The solvent was removed
by evaporation under reduced pressure,and the residue
was diluted with ethyl acetate (100 mL),washed with
water (75 mL · 2) and saturated NaCl solution (50 mL).
The organic layer was dried with magnesium sulfate
and filtered.The filtrate was evaporated at reduced
pressure,which was purified by silica gel column chromatography
with a gradient elution of ethyl acetate/n-hexane
to afford a white solid in 20.5–92.5% yield.Utilizing the
same procedure,ninety-six compounds were synthesized.