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ChemicalBook CAS DataBase List 4-Cyano-4-(dodecylsulfanylthiocarbonyl)sulfanylpentanoic acid, min. 97%
870196-80-8

4-Cyano-4-(dodecylsulfanylthiocarbonyl)sulfanylpentanoic acid, min. 97% synthesis

5synthesis methods
-

Yield:870196-80-8 91%

Reaction Conditions:

in ethyl acetate for 16 h;Heating / reflux;

Steps:

2
Example 2 Preparation of 4-Cvano-4-( dodecvlsulfanvth iocarbonvl)sulfanvl Pentanoic Acid ; A 2 liter, 3-neck flask fitted with reflux condenser, solids addition port, thermowell, and stir bar was charged with bis (dodecylsulfanylthiocarbonyl) disulfide (84.1 g, 151.6 mmol) ana 760 mL ethyl acetate. The resulting solution was heated to gentle reflux and reacted with 4,4'-azobis(4-cyanopentanoic acid) (72.1 g, 257 mmol) (Wako Chemicals USA, Inc. , Richmond, VA) over 3.75 h. The reaction mixture was heated for an additional 16 h. Ethyl acetate was removed under reduced pressure and the product was allowed to crystallize from heptane. The solid was filtered, washed with water, and dried to provide 110.0 g (91%). ¹H NMR (CDC13): 3.31 (t, a = 2.00), 2.72 to 2.61 (m) and 2.58 to 2.34 (AB, pattern with additional coupling, combined a = 3.96), 1.87 (s, a = 2.94), 1.68 (m, a = 2.02), 1.42 to 1.20 (overlapping CH2 signals, a= 18.62), 0.87 (t, a = 3.07), bd acid peak at ca. 10.0. Purity > 99%. ¹3C NMR (CDC13): 216.91 (C=S), 177.52 (C02H), 118.96 (CN), 46.38, 37.24, 33.65, 32.01, 29.72 (overlapping signals), 29.68,29.64, 29.52,29.43, 29.17,29.03, 27.79, 24.97, 22.78, 20.12, 14.20.

References:

E.I. DUPONT DE NEMOURS AND COMPANY WO2005/113493, 2005, A1 Location in patent:Page/Page column 3; 4-5

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