반응 #4287
ord-cc9151e5ad6b4f33b85396bdbeeebe64
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도with cooling in an ice bath
- 2여과filtered
- 3기타Solvent was removed from the filtrate in a rotary evaporator
- 4기타to give an oil which
- 5기타crystallized
- 6기타A portion was recrystallized from isopropyl ether
- 7기타to give white crystalline solid, m.p. 53°-55° C.
실험 절차
To a solution of 117.97 g (0.53 mole) of 2-[(3,4-dichlorophenyl)thio]ethanol (prepared by reacting 3,4-dichlorothiophenol and 2-chloroethanol) and 53.5 g (0.53 mole) of triethylamine in 500 ml of benzene was added dropwise a benzene solution of 60.9 g (0.53 mole) of methanesulfonyl chloride over a one hour period with cooling in an ice bath. The reaction mixture was stirred at room temperature overnight and filtered. Solvent was removed from the filtrate in a rotary evaporator to give an oil which crystallized. A portion was recrystallized from isopropyl ether to give white crystalline solid, m.p. 53°-55° C.