All the compounds prepared had high boiling points, and preliminary experiments showed that it would be necessary to use a column that would maintain a high reflux ratio if good fractionation was to be accomplished. Two columns were used. One was 81 cm. from bottom outlet to side arm, the other 46 cm. Both were 2.5 cm. in internal diameter, the longer having a bottom outlet of 12 mm. internal diameter, and the shorter a bottom outlet of 19 mrn. ...
