Reacción #1884962
ord-898e242162d8486fb5e3eaee4ead7238
Ecuación de reacción
tert-Butylamine
3-Chloropropanesulfonyl chloride
→
product
Rendimiento 99.0%
N-tert-Butyl-(3-chloro)propylsulfonamide
Rendimiento 99.0%
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1TemperaturaThe solution was cooled to −200C
- 2FiltraciónThe mixture was filtered
- 3Concentraciónthe filtrate was concentrated in vacuo
- 4workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
- 5LavadoThe resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
- 6Secadodried over Na2SO4
- 7FiltraciónIt was filtered
- 8Concentraciónconcentrated in vacuo
- 9Otroto give a slightly yellow solid, which
- 10Otrowas crystallized from hexane
Procedimiento
tert-Butylamine (3.0 mol, 315.3 mL) was dissolved in THF (2.5 L). The solution was cooled to −200C. 3-Chloropropanesulfonyl chloride (1.5 mol, 182.4 mL) was added slowly. The reaction mixture was allowed to warm to rt and stirred for 24 h. The mixture was filtered, and the filtrate was concentrated in vacuo. The residue was dissolved in CH2Cl2 (2.0 L). The resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L) and dried over Na2SO4. It was filtered and concentrated in vacuo to give a slightly yellow solid, which was crystallized from hexane to afford the product as a white solid (316.0 g, 99%).