تفاعل #1884962

معادلة التفاعل

tert-Butylamine

3-Chloropropanesulfonyl chloride

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product

المردود 99.0%

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

المردود 99.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was cooled to −200C
2. 2
   ترشيحThe mixture was filtered
3. 3
   تركيزthe filtrate was concentrated in vacuo
4. 4
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
5. 5
   غسيلThe resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
6. 6
   تجفيفdried over Na2SO4
7. 7
   ترشيحIt was filtered
8. 8
   تركيزconcentrated in vacuo
9. 9
   أخرىto give a slightly yellow solid, which
10. 10
    أخرىwas crystallized from hexane

الإجراء التجريبي

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%).

المصدر