反应详情

温度

80 °C

(E)-2-Chloro-6-(methylthio)benzaldehyde oxime (12.37 g) was dissolved in toluene (35 mL). Sulfuryl chloride (5.4 ml, 66.24 mmol) was added, dropwise to the solution at 0° C., followed by heating at 80° C. for 1 h. After the completion of the reaction, the reaction mixture was cooled to room temperature and a white precipitate formed. The solid was collected by vacuum filtration, washed with toluene and air dried to 4-chlorobenzo[d]isothiazol-3(2H)-one (6 g). (This method is general for other 2-(methythio) benzaldehyde oximes.) 1H NMR (300 MHz, DMSO-d6): 7.90 (t, 1H), 7.55 (t, 1H), 7.41 ppm (d, 1H). MW=186 confirmed by LC-MS, tr=2.38 min (Method B) MH+=187.

1. customAfter the completion of the reaction
2. temperaturethe reaction mixture was cooled to room temperature
3. customa white precipitate formed
4. filtrationThe solid was collected by vacuum filtration
5. washwashed with toluene and air
6. dry with materialdried to 4-chlorobenzo[d]isothiazol-3(2H)-one (6 g)
7. customconfirmed by LC-MS, tr=2.38 min (Method B) MH+=187