chloro-benzoyl chloride impurity or assay method

[dxydxyok]

Could anybody instruct me how to conduct the test for chloro-benzoyl chloride impurity or assay.

As an acyl halide, it is found easily to be hydrolyzed.So I try with normal liquid chromatography, but the results are not good.

I also try with GC method, but I am not sure whether this substance will react with GC phase or not because this is a very active substance.

Very thanks for your kind helps.

[SIELC_Tech]

Even at normal phase conditions acetyl chloride can react either with -OH of slica or traces of wate in you organic solvent. This will result in tailing as your compoun will hydrolize to acid. You can try to add ammonia or other amine to convert your acetyl chloride to amide. Reatction is very fast and goes almost 100%.

[james little]

Diethylamine would work well. We use a lot and analyze by GCMS and GC.

Since the acid is usually the impurity, dissolve your sample in DMF with diethylamine. Then after letting that react at 70C for 15 minutes, add BSTFA to silylate the acid which would be present.

Can get some artifacts with this method, I talk about them on my Web page.

see silylation section at

http://users.chartertn.net/slittle/

[dxydxyok]

Very thanks for the above!


Further to my queries, can we inject chloro-benzoyl chloride directly into the GC column with the normal used phases such as G27(5% phenyl-95% methylpolysiloxane) or G43(6% cyanopropylphenyl -94% dimethylpolysiloxane)?Is there any reaction happen?

Thanks again.

[james little]

The method I referred to in my note is commonly used in our GC group for alkylsulfonyl chlorides and acid chlorides. I normally just identify the components using GCMS for them.

As I remember, they had troubles trying to analyze directly.

[dxydxyok]

Very thanks!

Coluld you please favor me one example for my reference.

I need it very very urgent!

Please help!