ORGLIST: Re: Everybody Digest, Vol 18, Issue 3

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From: Krupa Shukla (krupa_shukla$##$yahoo.com)
Date: Fri Feb 03 2006 - 17:56:45 EST

Next message: Jon Kremsky: "ORGLIST: Aryl sulfides"
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use d1 to change relaxation time (increase to 5 or 6 s). I did for aromatic protons and it does work. give a shot.

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Today's Topics:

1. RE: Everybody Digest, Vol 18, Issue 2 (Ravi Orugunty)
2. Reductive Amination (shrent)
3. 2-BHP (Kishore Babu Ch)
4. ETHER SULFATE - hygroscopic ? (fine chem)
5. RE: Li-HMDS (Huan liang)

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Message: 1
Date: Thu, 2 Feb 2006 13:16:46 -0500
From: "Ravi Orugunty"
Subject: ORGLIST: RE: Everybody Digest, Vol 18, Issue 2
To:
Cc: esprcorn$##$hotmail.com
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Hi Ken,
This is with regards to the formates bound to the Pt, all of the
explainations seem valid. To explain differences in relaxations times as
well as D/H exchange use a different solvent such as d6DMF or d6DMSO or
CDCl3. there should be no exchange in these solvents and therefore should
integrate correctly. Try increasing the delay time while acquiring the
spectrum as well ( cant remember if it is the d1 or d2 delay, ask your
friendly NMR guru he will be able to help) and this will answer your
question of differences in relaxation times as well.
Of course the best and unequivocal evidence would be an X-ray of the
compound i.e if it is crystalline and you are able to grow good crystals.
good luck and let us informed about your results.
ravi

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Subject: Everybody Digest, Vol 18, Issue 2

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Today's Topics:

1. Li-HMDS (Kishore Babu Ch)
2. Postdoc position (Luisa Ferreira)
3. Vacancy Pharmachem, dehradun (saurabh vijay)
4. Re: Li-HMDS (Uno Maeorg)
5. Formate NMR (Ken Knott)

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Message: 1
Date: Tue, 31 Jan 2006 20:34:25 -0800 (PST)
From: Kishore Babu Ch
Subject: ORGLIST: Li-HMDS
To: everybody$##$orglist.net
Message-ID: <20060201043425.83077.qmail$##$web50608.mail.yahoo.com>
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Hi friends,

I anybody suggest how to prepare the lithium-HMDS.

bye
ch.k

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Message: 2
Date: Wed, 01 Feb 2006 14:00:43 +0000
From: Luisa Ferreira
Subject: ORGLIST: Postdoc position
To: everybody$##$orglist.net
Message-ID: <7.0.0.16.0.20060201135026.01c40d98$##$dq.fct.unl.pt>
Content-Type: text/plain; charset="iso-8859-1"

Postdoctoral position

One postdoctoral position is available to work on
semisynthesis of alkaloids.This position will be
available in early 2007. The application should be completed till June 2006.

Information

Lumsa Ferreira
REQUIMTE Departamento de Qu mmica,
FCT-UNL
2829-516 Caparica
Portugal
Tel.: 351 21 2948300
Fax.: 351 21 294 8550

Email: lpf$##$dq.fct.unl.pt
www.dq.fct.unl.pt
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Message: 3
Date: 1 Feb 2006 17:48:02 -0000
From: "saurabh vijay"
Subject: ORGLIST: Vacancy Pharmachem, dehradun
To: everybody$##$orglist.net
Message-ID: <20060201174802.8716.qmail$##$webmail64.rediffmail.com>
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Hi friends,

There is a vacancy available in Dolphin PG institute dehradunIndia, for the
post of Lecturer (M.Sc.with research exp. Or PhD. If you wish to apply,
please forward your resume to vj_saurabh$##$rediffmail.com

Thanks
Saurabh
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Message: 4
Date: Thu, 02 Feb 2006 01:15:49 +0200
From: Uno Maeorg
Subject: Re: ORGLIST: Li-HMDS
To: Kishore Babu Ch , everybody$##$orglist.net
Message-ID: <6.1.1.1.0.20060202011440.01e80e88$##$mega.chem.ut.ee>
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Hi,
This is well described in Lambert Brandsma's or Manfred Schlosser's new
book.

Uno

06:34 1.02.2006, Kishore Babu Ch wrote:
>Hi friends,
>
>I anybody suggest how to prepare the lithium-HMDS.
>
>bye
>ch.k
>
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Message: 5
Date: Wed, 01 Feb 2006 18:30:02 -0500
From: "Ken Knott"
Subject: ORGLIST: Formate NMR
To: everybody$##$orglist.net
Message-ID:
Content-Type: text/plain; format=flowed

So I've got two formates boud by the oxygen to a Pt... and the adehydic
protons aren't integrating correctly. They should be integrating to 2 as
their are 2 of them... however, they integrate closer to one in several
variants of the compound. All other characterizations indicate that the
compound is correct. Mass spec is exact and the elemental analysis is
correct other than some small error in the H% which seems to be normal...
HPLC show it's 99.5% pure as well.

How can I explain the incorrect integration of the formate H? NMR's have
been done in both CD3OD and D2O.

It has been suggested that it may be exchanging with the D's...
It has been suggested that is may be acidic....
It has been suggested that the spin relaxation rate of those protons may be
different that those of the pyridine protons it's being integrated against
due to the close proximity of the Pt.

Can anyone offer any other suggestions or comments on those above? Possible
experiments to conduct to explain the integration deviance?

Thanks,

Ken

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End of Everybody Digest, Vol 18, Issue 2
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Message: 2
Date: 3 Feb 2006 04:05:42 -0000
From: "shrent"
Subject: ORGLIST: Reductive Amination
To: everybody$##$orglist.net
Message-ID: <20060203040542.27685.qmail$##$webmail61.rediffmail.com>
Content-Type: text/plain; charset="iso-8859-1"

?lt;br>Hi !

Can I get advices regarding Direct conversion of a methyl-cyclo-aliphatic Ketone to its Primary Amine with commercial reagents ? It is based on Reductive Amination.

Awaiting your suggetions !

Regards,
shrent
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Message: 3
Date: Fri, 3 Feb 2006 03:12:25 -0800 (PST)
From: Kishore Babu Ch
Subject: ORGLIST: 2-BHP
To: everybody$##$orglist.net
Message-ID: <20060203111225.84480.qmail$##$web50606.mail.yahoo.com>
Content-Type: text/plain; charset=iso-8859-1

Dear friends,

If anybody suggest how to prepare the
2-bromo-3-hydroxy pyridine from 2-bromo-3-amino
pyridine .give any literature.

bye
ch.k

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Message: 4
Date: Thu, 2 Feb 2006 23:05:39 -0800 (PST)
From: fine chem
Subject: ORGLIST: ETHER SULFATE - hygroscopic ?
To: everybody$##$orglist.net
Message-ID: <20060203070539.55751.qmail$##$web34205.mail.mud.yahoo.com>
Content-Type: text/plain; charset="iso-8859-1"

Dear All,

Can someone please tell me if ETHER SULFATES are hygroscopic or not ?
It is actually an Alkyl ethylene oxide that has been sulfated and neutralized by base.
The product has an Alkyl chain length of C13 - C15, Also has an ethylene oxide moiety of EO = 3, and is a sodium salt.
Thanks in advance,

jmarjorie

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Message: 5
Date: Fri, 03 Feb 2006 01:02:09 -0800
From: "Huan liang"
Subject: RE: ORGLIST: Li-HMDS
To: kbchilukuri$##$yahoo.com, everybody$##$orglist.net
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hi,there,
1. lhmds you could buy it. I use it w/o any problems.
2. someone suggests to prep in situ.
To a cold solution of 111333-hexamethyldisilazane(1.8 eq) in dry THF was
added in nbuli (1.5eq). @-78C stir 45 mins. Then use it.

cheers.

LIANG, HUAN (steven)

----Original Message Follows----
From: Kishore Babu Ch
To: everybody$##$orglist.net
Subject: ORGLIST: Li-HMDS
Date: Tue, 31 Jan 2006 20:34:25 -0800 (PST)

Hi friends,

I anybody suggest how to prepare the lithium-HMDS.

bye
ch.k

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End of Everybody Digest, Vol 18, Issue 3
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