LC-MS check, column chromatography, HRMS check

Today I did it!

The hydrolysis of a very stable diethyl-acetal with 2M hydrogenchloride worked (THF, 2 h, reflux) and the following intramolecular cyclisation of a beta-ketoamide with the now deprotected aldehyde worked as well. LC-MS reactioncontroll is a really helpfull tool to get quick information about a conversion. I proceeded to check wether the compund is TLC stable or not by simple 2D-TLC. Yes! It is! Quickly ran a column with HRMS-analysis of the collected Spot. Perfect! It´s a mixture of three compounds with nearly the same Rf-value ! The cyclised compound, the cyclised compound including elimination of the newly formed alcohol and traces of my final compound! Tomorrow I will give sodiumhydroxide another chance to give me the cyclised and eliminated compound.  Then it is just one step away from the total synthesis of…..

I just want you to participate in this progress and I want to show, how emotional chemistry can be. More details regarding the synthesis strategy and the final product will follow as soon as possible.


Stay tuned 😉



Kommentar verfassen

Trage deine Daten unten ein oder klicke ein Icon um dich einzuloggen:

Du kommentierst mit Deinem Abmelden /  Ändern )

Google+ Foto

Du kommentierst mit Deinem Google+-Konto. Abmelden /  Ändern )


Du kommentierst mit Deinem Twitter-Konto. Abmelden /  Ändern )


Du kommentierst mit Deinem Facebook-Konto. Abmelden /  Ändern )


Verbinde mit %s