2,2-Dithiobis(pyridine-N-oxide) (1) was prepared by reacting 2-pyridinethiol-N-oxide (2) and hydrogen peroxide-urea adduct (3) at the molar ratio of 1:1.25 and 45oC for 1.75h in high yield and purity of 91.6% and 99.6% respectively. The structures of product were characterized by IR, NMR.
O-nitrotoluene is condensed with N, N-dimethylformamide dimethyl acetals in the presence of piperidine and DMF to yield trans-β-dimethylamino-2-nitrostyrene which undergoes hydrolysis in the 18% HCl aqueous solution to obtain o-nitrophenylacetaldehyde with yield of 83% and purity of 98.1% respectively.
1,1-Bis(hydroxymethyl)cyclopropane was synthesized by reaction dibromoneopentyl glycol with zinc powder at mole ratio of nDG:nzinc=1:1.05 and 80oC (slightly reflux) for 7 hours. Under optimal conditions, yield and purity of the title compound were 87.3% and 98.67%, respectively. Dibromoneopentyl glycol was also prepared in 91.7% yield with pentaerythritol and hydrobromic acid as material and diethyl sulfate as catalyst under reflux for 10 hours. Structural characterization of 1,1-bis(hydroxymethyl)cyclopropane was conducted by IR and H-NMR.
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