[ABA2015]

hi
I'm trying to synthesis nordazepam, which is synthesized from 2-amino-5-chloro-benzophenone and glycine ethyl ester hydrochloride in pyridine, it must be distilled with pyridine (and the fresh pyridine should be added to reaction mixture) to collect 2.5 times of the pyridine, I have performed the reaction 2 times and I have the same product with a big different in their purity , at first I tried to perform all the reaction process in one day, the obtained product was simply purified with benzene and petroleum ether and washing with acetone.
but in the second time I did the same but in 2 day, I mean I had to turn off the heater and continue the process tomorrow, I gained the same product but I can not purify it as simply as the first, when I wash it with the mentioned solvents above I obtain a solid with white and orange particles, the orange particles was not dissolved in acetone or benzene and petroleum ether, what should I do? 

[kriggy]

First, I woult analyze the orange particles by MS or other techniques and try to figure out what it is

[ABA2015]

First, I woult analyze the orange particles by MS or other techniques and try to figure out what it is

unfortunately we can't pay any analyze for impurities (due to our shortages) but the TLC shows the spot of desired product and another spot that is less polar.

[kriggy]

Then its going to be very hard to find out. Maybe if you can post the whole procedure

[TheUnassuming]

Might want to read the forum rules when it comes to discussing the synthesis of drugs, especially controlled ones that are prone to abuse. 
If you are somewhere that should be making this compound you should have access to a mass spec or other analytical means to determine what is going on. 

[Arkcon]

Might want to read the forum rules when it comes to discussing the synthesis of drugs, especially controlled ones that are prone to abuse. 
If you are somewhere that should be making this compound you should have access to a mass spec or other analytical means to determine what is going on.

Nicely summarized, *Thread Locked*

Listen people, when you want to learn about organic chemistry reactions, try to pick a general one, that involves the functional groups that you need to know about.

When you want to learn about purification techniques, again, work with logical procedures based on your reagent at hand.

Once you have both, you'll be able to make pretty much anything, and you won't have to come here asking for the specifics on this product or that product.