From: Anand Pandey (anand.pandey$##$alembic.co.in)
Date: Mon Jun 25 2007 - 23:36:56 EDT
Dear Christopher Luus,
Following methods you can try for,
1. Dilution with water and extraction with Diethylether (ether does not
holds dmf with water).
2. Azeotropic removal of dmf with xylenes. The azeotropic mixture of
xylenex contains ~17%dmf.
It is worth trying. Good Luck.
Regards
ANAND PANDEY
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Today's Topics:
1. Re: NH silica gel (Manjunath Channapur)
2. Removal of DMF. (Christopher Luus)
3. Re: Removal of DMF. (Richard Prankerd)
4. looking for a japanese scientist (samarium Steiner)
5. Re: Removal of DMF. (Ohad Ilovich)
6. Re: Removal of DMF. (Michael Engel)
----------------------------------------------------------------------
Message: 1
Date: Fri, 22 Jun 2007 12:10:54 +0530
From: "Manjunath Channapur" <channapur$##$gmail.com>
Subject: Re: ORGLIST: NH silica gel
To: Dr.Tushar <rajtush$##$yahoo.com>
Cc: everybody$##$orglist.net
Message-ID:
<f714e0590706212340s7ce6eb76qea54c14522769c48$##$mail.gmail.com>
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Dear Tushar
this may be silica is treated with aminepropyl trimethoxy silane.It is
also called SILNH2.
Regards
Manjunath B C
Scientist(synthetic chemistry)
Bangalore
On 6/20/07, Dr.Tushar <rajtush$##$yahoo.com> wrote:
> Anybody knows what is NH silica gel. I am sure it is not a neutral
silica
> but something different.
>
> Dr.Tushar
>
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-- Manjunath------------------------------
Message: 2 Date: Mon, 25 Jun 2007 11:41:45 +1000 From: "Christopher Luus" <cluu0433$##$mail.usyd.edu.au> Subject: ORGLIST: Removal of DMF. To: <everybody$##$orglist.net> Message-ID: <20070625014151.8641110FE28$##$mailwash35.pair.com> Content-Type: text/plain; charset="us-ascii"
Can anyone recommend an effective way of removing DMF from a crude reaction mixture? We have tried evaporation at high temperatures and low pressure using a rotovap to no avail.
Any suggestions would be greatly appreciated.
Thanks in advance,
Christopher Luus.
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Message: 3 Date: Mon, 25 Jun 2007 12:16:19 +1000 From: Richard Prankerd <Richard.Prankerd$##$vcp.monash.edu.au> Subject: Re: ORGLIST: Removal of DMF. To: Christopher Luus <cluu0433$##$mail.usyd.edu.au>, everybody$##$orglist.net Message-ID: <89907EA1DCFB7548A431C13A270F9DD501660C8F$##$prk-exch-01.vcp.local> Content-Type: text/plain; charset="iso-8859-1"
Christopher:
DMF can be removed with a rotovap, if the following precautions are taken: (a) the seal around the rotating shaft must be checked and freshly sealed with good quality vacuum grease; (b) vacuum must be from a mechanical pump in good condition, pulling < 0.5 mmHg; (c) the rotating flask must be heated to over 100 deg C; (d) the receiver must be cooled with ice water.
Removal can still be slow.
Richard
-----Original Message----- From: everybody-bounces$##$orglist.net on behalf of Christopher Luus Sent: Mon 6/25/2007 11:41 AM To: everybody$##$orglist.net Subject: ORGLIST: Removal of DMF. Can anyone recommend an effective way of removing DMF from a crude reaction mixture? We have tried evaporation at high temperatures and low pressure using a rotovap to no avail.
Any suggestions would be greatly appreciated.
Thanks in advance,
Christopher Luus.
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Message: 4 Date: Mon, 25 Jun 2007 07:47:03 +0200 From: "samarium Steiner" <neptunium$##$gmx.net> Subject: ORGLIST: looking for a japanese scientist To: everybody$##$orglist.net Message-ID: <20070625054703.267100$##$gmx.net> Content-Type: text/plain; charset="us-ascii"
Dear all
I am looking for a japanese scientist, preferably a chemist, who could help me translating a paper. I have a very old paper written in japanese from the journal "Yakugaku Zasshi" from the 19th century. It concerns the isolation of some natral ingredients and probably some chemical reactions thereof. I do not need an exact translation of the whole paper but I need to know whether there is mentioned a certain compound. The database SciFinder does not go back so early in the citations of Yakugaku zasshi.
Thank you very much,
samarium
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Message: 5 Date: Mon, 25 Jun 2007 09:21:10 +0200 From: "Ohad Ilovich" <ilovich$##$pob.huji.ac.il> Subject: Re: ORGLIST: Removal of DMF. To: <everybody$##$orglist.net> Message-ID: <000e01c7b6f9$67d93ab0$0e33a8c0$##$CYCLO14> Content-Type: text/plain; charset="iso-8859-1"
I've done it in two ways: 1) use an oil pump which gives better vacuum on the rotovap. if you don't have one though it'll be costly to buy one 2) dilute the reaction with water (approx. ten times the volume of DMF you have) and then extract the organic material with DCM or EtOAc or whatever you usually use Good luck, Ohad ----- Original Message ----- From: Christopher Luus To: everybody$##$orglist.net Sent: Monday, June 25, 2007 3:41 AM Subject: ORGLIST: Removal of DMF.
Can anyone recommend an effective way of removing DMF from a crude reaction mixture? We have tried evaporation at high temperatures and low pressure using a rotovap to no avail.
Any suggestions would be greatly appreciated.
Thanks in advance,
Christopher Luus.
------------------------------------------------------------------------ ------
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Message: 6 Date: Mon, 25 Jun 2007 12:16:41 +0900 (JST) From: "Michael Engel" <mkengel$##$gmail.com> Subject: Re: ORGLIST: Removal of DMF. To: everybody$##$orglist.net Message-ID: <1034739.56129.XAMJXAlJE1M=.1182741401.squirrel$##$webmailer.hosteurope.de> Content-Type: text/plain;charset=iso-2022-jp
> Can anyone recommend an effective way of removing DMF from a crude > reaction > mixture? We have tried evaporation at high temperatures and low pressure > using a rotovap to no avail.
Is adding the mixture to water an option ?
Cheers Michael
------------------------------
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End of Everybody Digest, Vol 35, Issue 12 *****************************************
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