反应 #1884962

反应方程式

tert-Butylamine

3-Chloropropanesulfonyl chloride

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product

收率 99.0%

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

收率 99.0%

溶剂

THF

反应条件

后处理

1. 1
   温度The solution was cooled to −200C
2. 2
   过滤The mixture was filtered
3. 3
   浓缩the filtrate was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
5. 5
   洗涤The resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
6. 6
   干燥dried over Na2SO4
7. 7
   过滤It was filtered
8. 8
   浓缩concentrated in vacuo
9. 9
   其他to give a slightly yellow solid, which
10. 10
    其他was crystallized from hexane

实验过程

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%).

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