反応 #46074

反応方程式

tert-Butylamine

3-Chloropropanesulfonyl chloride

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product

収率 99.0%

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

収率 99.0%

溶媒

THF

反応条件

後処理

1. 1
   温度to warm to rt
2. 2
   ろ過The mixture was filtered
3. 3
   濃縮the filtrate was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
5. 5
   洗浄The resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
6. 6
   乾燥dried over Na2SO4
7. 7
   ろ過It was filtered
8. 8
   濃縮concentrated in vacuo
9. 9
   その他to give a slightly yellow solid, which
10. 10
    その他was crystallized from hexane

実験手順

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%).

出典