Реакция #703731

Уравнение реакции

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

ethylene oxide

→

Compound 84

Выход 50.2%

2,6-diethyl-1-(2-hydroxyethyl)-2,3,6-trimethyl-4-piperidyl methylcarbamate

Выход 50.2%

Растворители

methanol

Условия реакции

Обработка

1. 1
   Концентрированиеthe reaction mixture was concentrated by evaporation under reduced pressure
2. 2
   Другоеthe residue was purified by column chromatography on silica gel using a 1 : 1
3. 3
   workup.ADDITIONby volume mixture of benzene and ethyl acetate as eluent

Методика

To a solution of 5.1 g of 2,6-diethyl-2,3,6-trimethyl-4-piperidyl methylcarbamate (Compound 66 - prepared as described in Preparation 4) in 8 ml of methanol were added 1.74 g of ethylene oxide and 1 drop of concentrated hydrochloric acid. The mixture was heated overnight at 100° C in a sealed tube. When the reaction was complete, the reaction mixture was concentrated by evaporation under reduced pressure and the residue was purified by column chromatography on silica gel using a 1 : 1 by volume mixture of benzene and ethyl acetate as eluent, giving 3.0 g of Compound 84. The compound showed a single spot on thin layer chromatography on silica gel (developing solvent: benzene/ethyl acetate, 1 : 1 by volume), Rf value 0.51.

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