Reaktion #1884962

Reaktionsgleichung

tert-Butylamine

3-Chloropropanesulfonyl chloride

→

product

Ausbeute 99.0%

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

Ausbeute 99.0%

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was cooled to −200C
2. 2
   FiltrationThe mixture was filtered
3. 3
   Einengenthe filtrate was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
5. 5
   WaschenThe resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
6. 6
   Trocknendried over Na2SO4
7. 7
   FiltrationIt was filtered
8. 8
   Einengenconcentrated in vacuo
9. 9
   Sonstigeto give a slightly yellow solid, which
10. 10
    Sonstigewas crystallized from hexane

Vorschrift

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%).

Quelle