Artisan Technology Group Quest 210 Specifications download pdf (Page 4)

polycarbonate capsules (ArgoCaps) are placed into the RVs and washed three times with

mL of dichloromethane (DCM). The efficient removal of the capsule by organic

solvent demonstrates the convenience of using ArgoCaps for solid-phase synthesis. After

performing a solvent exchange with anhydrous 1 -methyl-2-pyrrolidinone (NMP), PS-

DES

resin is allowed to react with a selection of alcohols and carbonyls (0.3

in NMP)

using Rl~cl(PPh~)~ as catalyst at

elevated temperature. The alcohol, carbonyls and

catalyst in NMP are conveniently delivered through the Luer Port of the Quest 21 0 upper

manifold under a low flow of nitrogen. RVs are pressurized with nitrogen to provide an

inert reaction environment for both alcoholysis and carbonyl hydrosilylation reactions.

After 3 h of heating at

60°C, the mixture is washed with solvent

via

a 4 L solvent bottle

connected to the Quest. This delivery system allows for parallel solvent delivery to 10

RVs simultaneously. The resin can be either dried for FT-IR analysis or carried forward

for the cleavage of the silyl ether. After cleavage and HF scavenging, products are

collected and concentrated for mass yield and GC analysis.

Note:

The results reported in

Table

(Page 28) at the end of this tutorial are

representative and your results may vary based on the purity of reagents used for

synthesis.

Instrument and Solution Preparation

Solution Preparation

RhCl(PPh3)3 solution in NMP (0.0075 M)

To a dry

mL pear-shaped flask containing a stir bar, add Rl~cl(PPh~)~ (76 mg,

0.082 rnrnol) under nitrogen. Add anhydrous NMP (1 1

mL)

to completely dissolve

the catalyst. Store the solution under nitrogen.

Alcohol or

carbon4 solution in NMP (0.3 M)

Prepare 4 mL of stock alcohol and carbonyl solutions as described in

Table

Store

the solution under nitrogen.

HFIpvridine solution in THF (0.4 M)

To a dry 100

pear-shaped flask containing a stir bar, add 40 mL of anhydrous

THF under nitrogen. While stirring, add 0.8 mL of pyridine followed

0.4

HFIpyridine (Aldrich, -70% HF, -30% pyridine). Store the solution under nitrogen.

Caution:

solutions should be handled with care in a fume hood.

Argonaut Technologies

Part

Number 102298

04/02/98

Quest Tutorial

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