반응 #46074

반응 방정식

tert-Butylamine

3-Chloropropanesulfonyl chloride

→

product

수율 99.0%

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

수율 99.0%

용매

THF

반응 조건

후처리

1. 1
   온도to warm to rt
2. 2
   여과The mixture was filtered
3. 3
   농축the filtrate was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
5. 5
   세척The resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
6. 6
   건조dried over Na2SO4
7. 7
   여과It was filtered
8. 8
   농축concentrated in vacuo
9. 9
   기타to give a slightly yellow solid, which
10. 10
    기타was crystallized from hexane

실험 절차

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%).

출처