Reaktion #1664058

Reaktionsgleichung

carbon tetrachloride

N-vinylsuccinimide

→

N-(1-chloroethyl)-succinimide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTION(0.40 mole) is dissolved in 1000 ml
2. 2
   Einengenwhile saturating with hydrogen chloride for 6 hours at 20° - 30°C
3. 3
   workup.WAITthe mixture is resaturated with hydrogen chloride for 1.5 hours
4. 4
   SonstigeAt the end of 48 hours, the solution is decanted
5. 5
   Waschenthe gummy residue is washed with ten 100 ml
6. 6
   Filtrationof diatomaceous earth, filtered
7. 7
   Einengenthe filtrate concentrated under reduced pressure to approximately 400 ml
8. 8
   FiltrationThe N-(1-chloroethyl)-succinimide is filtered
9. 9
   Sonstigedried at 20° - 30°C. under reduced pressure
10. 10
    Sonstigeto yield 38.4 g

Vorschrift

N-vinylsuccinimide, 50.0 g. (0.40 mole) is dissolved in 1000 ml. carbon tetrachloride, 5.20 g. (0.020 mole) of stannic chloride is added and the mixture is stirred while saturating with hydrogen chloride for 6 hours at 20° - 30°C. After 24 hours, the mixture is resaturated with hydrogen chloride for 1.5 hours. At the end of 48 hours, the solution is decanted and the gummy residue is washed with ten 100 ml. portions of carbon tetrachloride. The combined extracts are slurried with 10 g. of diatomaceous earth, filtered and the filtrate concentrated under reduced pressure to approximately 400 ml. The N-(1-chloroethyl)-succinimide is filtered and dried at 20° - 30°C. under reduced pressure to yield 38.4 g. (59%) of white solid melting at 83.5° - 84.5°C.

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