반응 #1478419

반응 방정식

2,6-diethyl-2,3,6-trimethyl-4-piperidinol

Compound 1

2,6-diethyl-2,3,6-trimethyl-4-piperidinol

methyl isocyanate

→

Compound 66

수율 97.2%

2,6-diethyl-2,3,6-trimethyl-4-piperidyl methylcarbamate

수율 97.2%

용매

xylene

반응 조건

후처리

1. 1
   온도the solution was refluxed
2. 2
   온도by heating for 3.5 hours
3. 3
   workup.DISTILLATIONXylene and excess methyl isocyanate were distilled off under reduced pressure
4. 4
   기타The residue was purified by column chromatography on silica gel ("60F 254", available from Merck & Co.)
5. 5
   workup.ADDITIONby volume mixture of chloroform and methanol as eluent
6. 6
   workup.DISTILLATIONThe product was then distilled under reduced pressure

실험 절차

4.0 g of 2,6-diethyl-2,3,6-trimethyl-4-piperidinol (Compound 1) and 1.7 g of methyl isocyanate were dissolved in 6 ml of xylene and the solution was refluxed by heating for 3.5 hours. Xylene and excess methyl isocyanate were distilled off under reduced pressure. The residue was purified by column chromatography on silica gel ("60F 254", available from Merck & Co.) using a 4 : 1 by volume mixture of chloroform and methanol as eluent. The product was then distilled under reduced pressure, giving 5.0 g of Compound 66 as a pale yellow liquid (bp 145°-149° C./1.4 mmHg).

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