反应详情

温度

100 °C

A suspension of 0.8 gram (0.011 mole) of sodium methanethiolate in 25 mL of DMF was stirred, and a solution of 1.8 grams (0.0044 mole) of 1,3-dichloro-5-methoxy-2-{4-[3-(trifluoromethyl)phenyl]piperazinyl}benzene in 40 mL of DMF was added. Upon completion of addition, the reaction mixture was heated to 100° C. where it stirred for two hours. After this time, the reaction mixture was cooled in an ice-water bath and 50 mL of water, followed by 25 mL of an aqueous solution of 10% hydrochloric acid, were added dropwise. The reaction mixture was then saturated with sodium chloride and extracted with two 50 mL portions of diethyl ether. The combined extracts were dried with sodium sulfate, filtered, and concentrated under reduced pressure to a residue. The residue was purified with column chromatography on silica gel using 1:1 methylene chloride:hexane, then 100% methylene chloride as eluants. The appropriate fractions were combined and concentrated under reduced pressure, yielding 1.1 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

1. additionUpon completion of addition
2. stirringstirred for two hours
3. temperatureAfter this time, the reaction mixture was cooled in an ice-water bath
4. additionwere added dropwise
5. extractionsaturated with sodium chloride and extracted with two 50 mL portions of diethyl ether
6. dry with materialThe combined extracts were dried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure to a residue
9. customThe residue was purified with column chromatography on silica gel using 1:1 methylene chloride
10. concentrationconcentrated under reduced pressure