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| 布雷德奈克試劑的典型應(yīng)用（2） |
| 2022-06-19 |
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A 50-L reactor is charged with intermediate (2) (7.25 Kg, 28.8 mol), DME (6.31 Kg),
and Bredereck's Reagent (7.7 Kg, 44.2 mole).
The solution is agitated and heated to 75° C.+-5° C. for at least three hours.
The progress of the reaction is monitored by HPLC.
The reaction is cooled to 0° C.+-5° C. over on hour during which time a precipitate forms
The mixture is held at 0° C.+-5° C. for one hour and filtered though a nutsche filter
and the product dried in a vacuum oven for at least 30 hours at 30° C.+-5° C.
to give intermediate (3) as a white crystalline solid (6.93 Kg, 77.9%).
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