Trace metals column crystallization

Diastereomer ratios were determined by gas chromatography. Since the aldol adduct undergoes retroaldol reaction on the column, it must be silylated prior to injection. Approximately 5 mg of the crude adduct is filtered through a short plug of silica gel to remove any trace metals. The material is taken up into 1-2 mL of dichloromethane in a 2-raL flask or small test tube. To this solution are added 4-5 drops of N,N-diethyl-1,1,1-trimethylsilylamine and a small crystal of 4-(N,N-dimethylamino)pyridine (Note 11), The solution is stirred for 2 hr and injected directly onto the column. (Column conditions 30 m x 0.32 mm fused silica column coated with OB 5, 14 psi hydrogen carrier gas, oven temperature 235°C). 

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