反应详情

Lithium hydroxide monohydrate (4.95 g) was added to a solution of methyl mercaptan (4.4 g) in N,N-dimethyl formamide, and 4-chloro-3-fluoro-2-(methylsulphenyl)benzoic acid (5.5 g) was added to the resultant mixture. It was stirred at room temperature for 1 hour and heated to 80° C. overnight. It was cooled, poured into water, extracted with ether, washed with water, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by column chromatography eluted with a mixture of acetic acid, ether and hexane (1:10:89) to give 2,3-bis(methylsulphenyl)-4-chlorobenzoic acid (3.24 g) as an off white solid, m.p. 130°-131° C.

1. temperatureheated to 80° C. overnight
2. temperatureIt was cooled
3. extractionextracted with ether
4. washwashed with water
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customThe filtrate was evaporated to dryness
8. customthe residue was purified by column chromatography
9. washeluted with a mixture of acetic acid, ether and hexane (1:10:89)