Reacción #8939
ord-771a37b166694f87a54ba1bf13c55b3c
Ecuación de reacción
1,3-benzodioxole
sulfuryl chloride
→
(1,3-benzodioxol-5-yl)sulfonyl chloride
Rendimiento 16.3%
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Otrowhereupon a solid formed
- 2TemperaturaThe reaction was cooled
- 3Extracciónextracted with methylene chloride
- 4Secadodried over magnesium sulfate
- 5Filtraciónfiltered
- 6Concentraciónconcentrated
- 7Otroto give 7.32 g of crude material as a black oil
- 8OtroThis was chromatographed on silica gel using 20% methylene chloride/hexane
Procedimiento
To a solution of 4.25 g of anhydrous N,N-dimethylformamide at 0° C. under nitrogen was added 7.84 g of sulfuryl chloride, whereupon a solid formed. After stirring for 15 minutes, 6.45 g of 1,3-benzodioxole was added, and the mixture heated at 100° C. for 2 hours. The reaction was cooled, poured into ice water, extracted with methylene chloride, dried over magnesium sulfate, filtered and concentrated to give 7.32 g of crude material as a black oil. This was chromatographed on silica gel using 20% methylene chloride/hexane to afford 1.9 g of (1,3-benzodioxol-5-yl)sulfonyl chloride.