反应详情

A solution of 2-[(3,4-dichlorophenyl)thio]ethanol (117.97 g, 0.53 mole) prepared from 3,4-dichlorothiophenol and 2-chloroethanol, in benzene (500 ml) with triethylamine (53.5 g, 0.53 mole) was prepared. To this solution was added dropwise a benzene solution of methanesulfonyl chloride (60.9 g, 0.53 mole) over 1 hr (in an ice bath). The reaction mixture was stirred at room temperature overnight and then filtered. Solvent was removed by evaporation to give an oil which crystallized. A 5 g portion was recrystallized from isopropyl ether to give 4.61 g (47.9% yield based on aliquot) of white crystalline solid, m.p. 53°-55° C.

1. customwas prepared
2. filtrationfiltered
3. customSolvent was removed by evaporation
4. customto give an oil which
5. customcrystallized
6. customA 5 g portion was recrystallized from isopropyl ether
7. customto give 4.61 g (47.9% yield based on aliquot) of white crystalline solid, m.p. 53°-55° C.