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Topic: How to handle an easily decomposing intermediate?  (Read 3603 times)

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Offline Bro-Mide

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How to handle an easily decomposing intermediate?
« on: December 07, 2011, 11:46:44 PM »
If you have an intermediate organic compound that decomposes quickly and easily what steps would you take to protect it from oxygen as you work on it to keep your yield high.

Offline discodermolide

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Re: How to handle an easily decomposing intermediate?
« Reply #1 on: December 08, 2011, 12:24:51 AM »
If you have an intermediate organic compound that decomposes quickly and easily what steps would you take to protect it from oxygen as you work on it to keep your yield high.

How do you know that oxygen is the problem? If that is the case keep it under nitrogen.
Keep your temperatures low, keep it in solution.
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Offline Bro-Mide

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Re: How to handle an easily decomposing intermediate?
« Reply #2 on: December 08, 2011, 01:52:13 AM »
Well I don't know it's because of oxygen. The procedure just says it decomposes easily especially if you try to further distill it. The longer you wait the more of it decomposes. I just wanted to know what techniques besides work faster would help.

Offline discodermolide

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Re: How to handle an easily decomposing intermediate?
« Reply #3 on: December 08, 2011, 02:34:56 AM »
Well I don't know it's because of oxygen. The procedure just says it decomposes easily especially if you try to further distill it. The longer you wait the more of it decomposes. I just wanted to know what techniques besides work faster would help.

Any idea of it's BPt.?
You can use flash distillation, spinning band distillation, molecular distillation etc. It would seem that you need a very good vacuum for this one.
If you can run a DSC to determine at which temperature the decomposition begins.
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Offline Bro-Mide

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Re: How to handle an easily decomposing intermediate?
« Reply #4 on: December 08, 2011, 02:44:06 AM »
BP is ~112 degrees C at 0.1mm. What is a DSC?

Offline discodermolide

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Re: How to handle an easily decomposing intermediate?
« Reply #5 on: December 08, 2011, 03:07:14 AM »
BP is ~112 degrees C at 0.1mm. What is a DSC?

A DSC is a differential scanning caliometery It allows you to measure MPts, BPts., energy of decomposition. It will tell you exactly the temperature when your compound starts to decompose.
That BPt you quoted is quite exact!
Try and get a better vacuum, use a diffusion pump. There are plenty of graphs available which let you determine the BPt. at various temperatures and pressures.
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