Benzene, 1-broMo-2-[(2,2-diMethoxyethyl)thio]- synthesis

Yield:799766-06-6 240 g

Reaction Conditions:

with potassium carbonate in acetone at 55; for 4 h;

Steps:

1

Potassium carbonate (260 g, 1.9 mmol) was added to a stirring solution of 2-bromobenzenethiol (180 g, 0.96 mol, Matrix Scientific, Columbia, SC), 2-bromo-l,l-dimethoxy ethane (170 g, 1.0 mol, Spectrochem, India), and acetone (1.8 L) at room temperature, and then the reaction mixture was heated at 55 °C. After 4 h, the reaction mixture was cooled to room temperature, filtered, the filter cake was washed with acetone, and the combined filtrate was concentrated under a vacuum. The residue was partitioned between ethyl acetate and water, the layers were separated, the organic material was washed with brine, dried (sodium sulfate), filtered, and the filtrate was concentrated under a vacuum to give l-bromo-2-((2,2-dimethoxyethyl)sulfanyl)benzene (240 g) as a pale yellow oil. The material was used in the next step of the synthesis without purification.

References:

WO2013/173382,2013,A1 Location in patent:Page/Page column 104