Jul-Aug 2003
Nickel Boride Mediated Reductive Desulfurization
679
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temperature. After complete disappearance of the starting material
as monitored by TLC (eluent – benzene:ethyl acetate::90:10;v/v),
the reaction mixture was filtered on pump through a celite pad
(~ 1 inch). Nickel boride precipitate was washed with methanol (2
x 10 mL). The combined filtrate was diluted with water (~ 50 mL)
and extracted with ethyl acetate (3 x 10 mL). The combined ethyl
acetate extract was dried over anhyd. MgSO4, filtered and concen-
trated under reduced pressure on a Büchi rotavapor to afford II or
III as indicated in Table 1. Analytically pure samples were
obtained by crystallization from ethanol or purified by column
chromatography (run 13) over silica gel (100-200) mesh using
benzene:ethyl acetate as eluent. The products were analysed by
mp, IR, NMR and mass spectra; IIb: 1H NMR (60MHz, CDCl3):
d 8.05 (s, 1H), 6.70-7.50 (m, 8H), 5.0 (s, 2H), 2.40 (s, 3H); MS
found : m/z: 238 (M+, 35 %); IIIb: 1H NMR (60MHz, CDCl3): d
7.0-8.5 (m, 9H), 2.45 (s, 3H); MS found : m/z: 236 (M+, 20 %).
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Acknowledgement.
We are pleased to acknowledge the financial support for this
work by CSIR, New Delhi, India, Project No. 01(1567)/99/EMR-
II. The author GK also wishes to thank CSIR for providing SRF.
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