2-PYRIDYLETHYL THIOLACETATE synthesis

Yield:59020-97-2 78.2%

Reaction Conditions:

at 5 - 20; for 2 h;Inert atmosphere;

Steps:

4-1-1

Into a 100-mL four-necked flask equipped with a nitrogen gas introduction tube, thermometer, Dimroth condenser, and dropping funnel was introduced 15.22 g (0.20 mol) of thioacetic acid (manufactured by Tokyo Kasei Kogyo Co., Ltd.). The contents began to be stirred, and nitrogen was introduced. Thereafter, the contents were cooled to 5°C or lower with an ice bath, and 21.03 g (0.20 mol) of 2-vinylpyridine was added dropwise thereto through the dropping funnel over 1 hour. After completion of the dropwise addition, the ice bath was removed, and the mixture was stirred at room temperature for further 1 hour and reacted. After completion of the reaction, the liquid reaction mixture was subjected to vacuum distillation under the conditions of a bath temperature of 120°C and a pressure of 0.8 kPa to obtain 27.8 g of 2-pyridylethyl thioacetate. As a result of analysis by gas chromatography, the 2-pyridylethyl thioacetate was found to have a purity of 96.8% and the yield thereof was found to be 78.2%. Conditions of the gas chromatography and the method used for calculating the yield are shown below.(Gas Chromatography) Apparatus: "GC-14A", manufactured by Shimadzu Corp.Column: "TC-5" (60 m × 0.32 mm × 1.0 μm), manufactured by GLSciencesDetector: FIDCarrier gas: helium

References:

EP2390243,2011,A1 Location in patent:Page/Page column 34