Методика

[ashpwnz]

Доброго времени суток. Несколько дней ищу, найти не могу ни одной методики по сшивке малеимида с тиолом. Буду крайне признателен, если поможете найти. Спасибо!

 

[tixmir]

Trost, Barry M.; Kallander, Lara S.
Journal of Organic Chemistry, 1999 , vol. 64, # 15 p. 5427 - 5435

 

General procedure: Into a round-bottom flask charged with a magnetic stirbar was added an appropriate Michael acceptor (1.0 equiv). This material was dissolved in enough EtOH to produce a 0.1 M solution. After stirring to ensure dissolution, mercaptan (1.0 equiv) was added, and the mixture was stirred until homogenous. After this time, TBA-OH (40wtpercent in H2O, 1 molpercent ) was added in one portion, and the mixturewas stirred until deemed complete by TLC analysis. The mixture was then partitioned between deionized H2O (50 mL) and Et2O (50mL). After removing the organic layer, the residual product was extracted from the aqueous layer using an additional portion of Et2O (50 mL). The combined organic layers were then washed with deionized H2O (50 mL) then brine (50 mL). After drying (MgSO4), the crude product was concentrated under reduced pressure, then, if necessary, purified via column chromatography.