반응 #80665

반응 방정식

epichlorohydrin

toluene

4-hydroxy-1,2,2,6,6-pentamethylpiperidine

sodium hydroxide

→

1,2,2,6,6-Pentamethyl-4-(2,3-epoxypropoxy)piperidine

용매

—

ice water

water

반응 조건

후처리

1. 1
   기타fitted with mechanical stirrer, condenser
2. 2
   기타the organic phase is separated off
3. 3
   기타dried
4. 4
   기타evaporated
5. 5
   workup.DISTILLATIONThe residue is distilled at 0.05 mmHg over a Vigreux column
6. 6
   기타the fraction of boiling point 71°-72° C. is collected

실험 절차

300 g (7.5 mol) of sodium hydroxide are dissolved in 300 g of water under an argon atmosphere in a 2.5 l sulfonation flask fitted with mechanical stirrer, condenser and 500 l dropping funnel. 750 ml of toluene, 48.4 g (0.15 mol) of tetrabutylammonium bromide and 257 g (1.5 mol) of 4-hydroxy-1,2,2,6,6-pentamethylpiperidine are added. 347 g of epichlorohydrin (3.75 mol) are added dropwise at 60° C. over the course of 1.5 hours, and the mixture is subsequently stirred at the same temperature for a further 4 hours. The reaction solution is poured in 3 l of ice water, and the organic phase is separated off, dried using sodium sulfate and evaporated. The residue is distilled at 0.05 mmHg over a Vigreux column, and the fraction of boiling point 71°-72° C. is collected. Yield: 205 g (60%). GC: >99%.

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