반응 #8728

반응 방정식

2,5-dichlorothiophene-3-sulfonyl chloride

sulfur monochloride

water

→

solid

2.4.5-Trichloro-thiophene-3-sulfonyl chloride

용매

sulfuryl chloride

sulfuryl chloride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   온도The reaction was heated at 60° C. for an additional 3 hours, at which time it
3. 3
   온도to cool to ambient temperature
4. 4
   추출the reaction extracted with dichloromethane (2×20 mL)
5. 5
   세척The combined organic layers were washed with saturated sodium bicarbonate solution
6. 6
   건조dried (Mg2SO4)
7. 7
   농축concentrated

실험 절차

A mixture of 2,5-dichlorothiophene-3-sulfonyl chloride (1.2 g, 5 mmol) and sulfur monochloride (10 mg) in sulfuryl chloride (500 mg) was heated at 60° C. for 30 min, at which time was added dropwise a mixture of aluminum trichloride (10 mg) in sulfuryl chloride (500 mg). The reaction was heated at 60° C. for an additional 3 hours, at which time it was allowed to cool to ambient temperature. Cold water (20 mL) was added and the reaction extracted with dichloromethane (2×20 mL). The combined organic layers were washed with saturated sodium bicarbonate solution, dried (Mg2SO4) and concentrated to furnish a tan solid (420 mg, 33%).

출처