Pergamon
Tetrahedron Letters, Vol. 38, No. 44, pp. 7681-7682, 1997
© 1997 Elsevier Science Ltd
All rights reserved. Printed in Great Britain
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Selective Hydroboration of Unconjugated Alkynyl
Ketones and Aldehydes
George W. Kabalka,* Su Yu and Nan-Sheng Li
Departmentof Chemistry;The Universityof Tennessee
Knoxville, TN 37996-1600
Abstract: Unconjugated alkynyl ketones and aldehydes are selectively
hydroborated to give the corresponding olefinic carbonyl compounds after
protonation, or dicarbonyl compounds after oxidation.
© 1997 Elsevier Science Ltd.
Hydroboration of alkenes and alkynes has been utilized extensively in organic synthesis. ~
The hydroboration of substrates containing carbonyl groups is often carried out by either
converting the carbonyl group to a less reactive functionality 2 or modifying the hydroborating
agent 3 to avoid reduction of the carbonyl group 4 even though kinetic studies involving
disiamylborane suggested that these approaches might not be necessary, s Recently, we
reported that terminal alkenes could be selectively hydroboreted in the presence of ketones and
aldehydes.6 We now wish to report the selective hydroboration of unconjugated alkynyl ketones
and aldehydes.
o
O
~ NaBO3 O O
= ~ (76%)
A variety of unconjugated alkynyl carbonyl compounds were hydroborated with
dicyclohexylborene. The results are summarized in the Table. Both terminal and internal alkynyl
carbonyl compounds could be selectively hydroboroated in the presence of the carbonyl group.
The reaction affords the corresponding olefins in high yields (71-94%) after protonation, or the
dicarbonyl compounds in good yields (50-76%) after oxidation with sodium perborate, z
The hydroboration of 11-dodecyn-2-one is representative: BH3-THF (2.0 mmol, 2.0 mL of
a 1.0M solution in THF) was placed in a dry, argon-flushed flask which was then immersed in an
ice-water bath. Cyclohexene (4.0 mmol, 0.33g, 0.41 mL) was added dropwise and the mixture
stirred at 0 °C for 1 hour. 11-Dodecyn-2-one (2.0 mmol, 0.36 g) was then added to the slurry of
dicyclohexylborane in THF. The cooling bath was removed and the mixture stirred for 1 hour at
room temperature. Protonation was achieved by adding glacial acetic acid (1 mL) and stirring
7681