sulfur; triethylamine; n,n-dimethyl-formamide; n,n-dimethyl-formamide;
reactants are commercially availlable.
ramot at tel-aviv university ltd, wo2008/50341, a2, (2008) for a general synthesis see he, x.; griesser, u. j.; stowell, j. g.; borchrdt, t. b.; byrn, s. r. j. pharm. sci. 2001, 90, 371.a sulfur (s8, 0.9 g, 0.0 27 mmol), propionalaldehyde (2 ml, 0.027 mmol) and dmf (6 ml) were transferred to a thre e-necked round-bottomed flask equipped with a dropping funnel and condenser. the resulting mixture was cooled to 0°c, and epo triethylamine (2.3 ml) was added in a dropwise manner via the dropping funnel. the resulting dark sol ution was then warmed to room temperature over a period of 1 h. a solution of malononitrile (1.71 ml, 1.8 g, 0.027 mmol) in dmf (3.2 ml) was transferred to the addition funnel and added in a dropwise manner. the resulting brownish mixture w as stirred overnight at room temperature. then the mixture was poured over 80 ml of ice and water to yield an orange precipitate. the solid a was filtered, washed with chilled water, and dried in vacuo; yield 78percent.1h nmr (200 mhz, cdcl 3): delta 6.35 (s, ih), 4.15 (br s, 2h), 2.27 (s, 3h). 13c nmr (50 mhz, cdcl3): delta 160.9, 146.3, 124.6, 122.0, 115.7, 14.9.
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