744 Letters in Organic Chemistry, 2006, 3, 744-748
1,2-Glycerol Carbonate: A Versatile Renewable Synthon
Ana-Catarina Simão
a,b
, Benita Lynikaite-Pukleviciene
a,c
, Cyril Rousseau
c
, Arnaud Tatibouët
*,a
,
Stéphanie Cassel
a
, Algirdas
Sackus
c
,
˘
˘
Amelia P. Rauter
b
and Patrick Rollin
*,a
a
I.C.O.A. - UMR 6005,Université d'Orléans, BP 6759, F-45067 Orléans, France
b
F.C.U.L. - Campo Grande, Edifício C5, Lisboa, Portugal
c
K.T.U. - Chemines
.
Technologijos Fakultetas, LT-50270 Kaunas, Lithuania
Received July 04, 2006: Revised October 03, 2006: Accepted October 03, 2006
Abstract: Activated 1,2-glycerol carbonate has been subjected to nucleophilic substitution with oxygen-,
nitrogen- and sulfur nucleophiles. Selective reactions with thiol derivatives have been especially investigated
for the preparation of mono- and dithiofunctionalized 3-carbon synthons.
Keywords: Glycerol carbonate, renewable resources, thiofunctionalization, oxidation.
INTRODUCTION been investigated using lipase-catalysed acetylation and/or
alcoholysis [5a]. More recently, self-condensation to
oligomers has been explored [6], but little has been
developed on chemical transformations of 2 when treated
with various nucleophiles. Our interest is focused on the
versatility of such an activated form of glycerol as a multi-
electrophilic synthon in which the primary hydroxyl group
can also be activated (Scheme 2). Glycerol carbonate might
Valorisation of glycerol 1 is becoming a crucial challenge
for industrial companies: this small molecule appears as a
major side-product during manufacturing of bio-diesels, fatty
acids and surfactants [1]. This abundant and renewable itol is
a prochiral C-3 synthon which has been widely investigated
and used as raw material [2]. Among the glycerol-based
O
O
O
HO OH
OH
HO
O
O
HO
O
O
HO
X
O
O
O
4
2
1
3
Nu
4 elec tes t rophil ic si
Scheme 1. Classical synthons from glycerol and proposed site reactivities of activated 1,2-glycerol carbonate.
cyclic acetals (Scheme 1), 1,2-O-derivatives have been
largely described and studied mainly as a source of chirality
[3]. In contrast to its ready accessibility [4], 1,2-glycerol
carbonate 2 has been scarcely studied as precursor for the
development of new synthons in organic chemistry [5].
thus be regarded as an alternative synthon to glycidol or
activated glycidols, with a highly reduced toxicity [7].
RESULTS AND DISCUSSION
Activation of the free alcohol function of 2 through
sulfonate formation using mesyl or tosyl chloride under
basic conditions gave 5 or 6 in 92% and 99% yield
respectively. No side-product was detected in the tosylation
process while predictable chloride ion counter-attack occurred
during mesylation, albeit in 6% yield only. Mesylate 5 was
used first to test the displacement with a few standard
nucleophiles (Table 1).
Compared to Solketal® (1,2-O-isopropylideneglycerol)
3, the reactivity potential of glycerol carbonate 2 is by far
more important. The resolution of racemic 2 has already
*Address correspondence to these authors at the I.C.O.A. – UMR 6005,
Université d'Orléans, BP 6759, F-45067 Orléans, France; Tel:
33(0)238417370; Fax: 33(0)238417281;
The preliminary results showed rather poor yields for a
selective nucleophilic mono-substitution (products 7-11a).
E-mail: patrick.rollin@univ-orleans.fr; arnaud.tatibouet@univ-orleans.fr
1570-1786/06 $50.00+.00 © 2006 Bentham Science Publishers Ltd.