3-BroMopyridine-2-thiol synthesis

Yield:65938-86-5 55%

Reaction Conditions:

Stage #1: 3-bromo-2-chloropyridinewith sodium sulfide in N,N-dimethyl-formamide at 130; for 0.5 h;Microwave irradiation;
Stage #2: with water pH=6;Acidic conditions;

Steps:

4A.C

[00287] Step C: 3-bromopyridine-2-thiolA mixture of 3-bromo-2-chloropyridine (0.769g, 4mmol) and sodium sulfide (0.336g, 6mmol) in DMF (3mL) was heated under microwave irradiation at 130°C for 0.5 hour. Water (50mL) and ethyl acetate (20mL) were added and the layers separated. The aqueous layer was acidified to pH 6 resulting in the formation of a precipitate, which was isolated by filtration and dried under vacuum to yield the product as a yellow solid (0.42g, 55%).

References:

WO2011/159839,2011,A2 Location in patent:Page/Page column 98