Реакция #703726

Уравнение реакции

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

Compound 1

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

methyl isocyanate

→

Compound 66

Выход 97.2%

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

Выход 97.2%

Растворители

xylene

Условия реакции

Обработка

1. 1
   Температураthe solution was refluxed
2. 2
   Температураby heating for 3.5 hours
3. 3
   workup.DISTILLATIONXylene and excess methyl isocyanate were distilled off under reduced pressure
4. 4
   ДругоеThe 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

Методика

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).

Источник