Reacción #46074

Ecuación de reacción

tert-Butylamine

3-Chloropropanesulfonyl chloride

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product

Rendimiento 99.0%

N-tert-Butyl-(3-chloro)propylsulfonamide

Rendimiento 99.0%

Disolventes

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturato warm to rt
2. 2
   FiltraciónThe mixture was filtered
3. 3
   Concentraciónthe filtrate was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
5. 5
   LavadoThe resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
6. 6
   Secadodried over Na2SO4
7. 7
   FiltraciónIt was filtered
8. 8
   Concentraciónconcentrated in vacuo
9. 9
   Otroto give a slightly yellow solid, which
10. 10
    Otrowas crystallized from hexane

Procedimiento

tert-Butylamine (3.0 mol, 315.3 mL) was dissolved in THF (2.5 L). The solution was cooled to −20° C. 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%).

Fuente