반응 #8729

반응 방정식

3-methylthiophene

dichloromethane

sulfuryl chloride

dichloromethane

chlorosulfonic acid

→

oil

수율 25.0%

2,5-Dichloro-4-methylthiophene-3-sulfonyl chloride

수율 25.0%

반응 조건

후처리

1. 1
   농축The reaction was concentrated
2. 2
   workup.DISSOLUTIONredissolved in dichloromethane (30 mL)
3. 3
   온도cooled to −10° C
4. 4
   온도The reaction was maintained at −10° C. for 30 minutes
5. 5
   workup.WAITat ambient temperature for 16 hours
6. 6
   추출extracted with dichloromethane (50 mL)
7. 7
   건조The organic layer was dried (Mg2SO4)
8. 8
   농축concentrated

실험 절차

To a cooled (10° C.) solution of 3-methylthiophene (5 g, 50 mmol) in dichloromethane (15 mL) was added a solution of sulfuryl chloride (8.6 mL) in dichloromethane (5 mL). The reaction mixture was maintained at 10° C. for 30 minutes, then at ambient temperature for 16 hours. The reaction was concentrated and redissolved in dichloromethane (30 mL) and cooled to −10° C. To the cooled solution was added chlorosulfonic acid (2 mL, 100 mmol). The reaction was maintained at −10° C. for 30 minutes, then at ambient temperature for 16 hours, at which time it was poured into ice water (50 mL) and extracted with dichloromethane (50 mL). The organic layer was dried (Mg2SO4) and concentrated to furnish a brown oil (3.3 g, 25%).

출처