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| General Procedure for Monitoring Solid-Phase Reactions. An aliquot of vacuum-dried resin (4 mg) was swollen with THF (5 mL) for 10 min. A solution of 4-methoxybenzylalcohol (internal standard) (25 mM in THF, 1 eq) was added, followed by tetra-n-butylammonium fluoride (0.1 M in THF, 3 eq). After stirring for 2 h, the THF solution was recovered from the resin, and the solution concentrated by rotary evaporation. The residue was taken up in CH3CN (300 ¦ÌL) and filtered through a Pasteur pipette with a 0.5-inch plug of normal phase silica gel over a 0.5-inch plug of reverse-phase silica gel. The plug was rinsed carefully with 3 mL CH3CN, and the crude cleavage products were recovered by rotary evaporation. HPLC analysis (ELSD) was used to determine the ratio of cleaved scaffold to internal standard, and the yield was calculated based on a calibration curve. Analysis by 1H-NMR was used to determine product ratios where appropriate. |
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ringzhu(½ð±Ò+1): O(¡É_¡É)O~ 2011-06-04 13:12:28
lgq101(½ð±Ò+10, ·ÒëEPI+1): лл~~~~ 2011-06-04 15:43:01
ringzhu(½ð±Ò+1): O(¡É_¡É)O~ 2011-06-04 13:12:28
lgq101(½ð±Ò+10, ·ÒëEPI+1): лл~~~~ 2011-06-04 15:43:01
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