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procedure.html
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<!DOCTYPE HTML PUBLIC "-//W3C//DTD HTML 4.01 Transitional//EN" "http://www.w3.org/TR/html4/loose.dtd">
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<meta http-equiv="Content-Type" content="text/html; charset=utf-8">
<title>Experimental</title>
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<center>
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<img src="images/title.png" alt="Anthony Sottile" title="Anthony Sottile">
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<center>
<a href="index.html"><img src="images/home.png" alt="Home"></a><br><br>
<a href="nmr.html"><img src="images/nmr.png" alt="NMR"></a><br><br>
<a href="procedure.html"><img src="images/procedure.png" alt="Procedure"></a><br><br>
<a href="mechanism.html"><img src="images/mechanism.png" alt="Mechanism"></a><br><br>
<a href="reference.html"><img src="images/reference.png" alt="References"></a><br><br>
<a href="leadingq.html"><img src="images/leadingq.png" alt="Leading Question TfOH"></a><br><br>
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<img src="images/proceduresub.png" alt="Experimental Procedure">
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<br><br>
<b>Compound 41</b> (14.4 mg, 0.049 mmol, 1.0 equiv.) was dissolved in dichloromethane (490 µL, 0.1 M) and cooled to 0 °C.
<u><span onmouseover="document.getElementById('deftext').innerHTML= '<img src=images/triflic.png alt=Triflic style=float:right;><b>Trimethylsilyltrifluoromethanesulfonate (aka Triflic acid or TfOH)</b> - An extremely strong sulfonic acid.<br>';" onmouseout="document.getElementById('deftext').innerHTML = 'Mouse Over an Underlined word for its definition';">Trimethylsilyltrifluoromethanesulfonate</span></u> (26.6 µL, 0.147 mmol, 3.0 equiv.) and MeOH (2.2 µL, 0.054 mmol, 1.15 equiv.) were added and the solution was stirred at 0 °C for one hour.
The reaction was then quenched by the addition of 5% Sodium Bicarbonate (2.0 mL) and diluted with Ethyl Acetate (4.0 mL).
The organic layer was washed with water (2.0 mL). Then it was washed with brine (2.0 mL) and then dried with MgSO4.
The solvent was removed by a vacuum.
This was then purified by flash column chromatography (silica gel, gradient from 3:1 hexanes:DCM to DCM) to give <b>compound 43</b> (4.4 mg, 31%) and recovered <b>compound 41</b> (8.5 mg, 59%).
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