
This experiment is performed according to literature method [1,2,3,4]. To a solution of bis[(3- methoxycarbonyl-5-methyl pyrazol)-1-yl thiocarbonyl] disulfide 1 (7.3x10-2mol) in dry diethyl ether was added a solution of LiAlH4 (2.78 g, 7.3x10-2mol) in 10 mL of dry ether. The mixture was stirred for 6h at 30 °C and the product was extracted with CHCl3 dried over Na2SO4 and filtred. The solvent was removed under reduced pressure and the product was dried under high vacuum.
Yield: (70%).
1H-NMR (DMSO) d (ppm): 2,16 (s, 6H, CH3); 4,33 (s, 4H, CH2); 5,86 (s, 2H CH).
13C-NMR (CDCl3) d (ppm): 193 (-C=S), 65 (CH2-OH).
IR (KBr , cm-1): 3300 (-S-S-); 1240 (C=S).
MS (m/z): 374 [M]+.
U.V.: lmax = 290 nm (-C=S).
References
- Jones, R.G.; Hanret, M.J.; Lauglin, K.M. J. Org. Chem . 1954, 19, 1428. [CrossRef]
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