temperature was 44 u00b0 c vol 8115 ml the solids were filtered off at 53 u00b0 c using isolated vacuum the filtration was quick and easy the reactor and wet cake were rinsed with warm 35 u00b0 c water 2 5 l and the filtrates were combined the wet cake was pulled dry for 15 20 minutes the two wet cakes 3587 g were dried under vacuum at 60 u00b0 c for 90 hours to give a dry wt of 1075 38 g crude compound 4 theoretical yield is 977 g __________________________________________________________________________chemicals source assay wt ml d mw mmol equiv__________________________________________________________________________crude compound 4 895 131 91 82 290 g 567 79 469 1 00acetone fisher 4038 g 5105 0 791 58 08water di 1070 g 1070 1 000 18 02celite aldrich 29 gdarco g 60 activated fisher 44 g 12 01carbon__________________________________________________________________________ a 12 liter 3 neck rbf fitted with a condenser temperature probe and mechanical stirrer was charged with crude compound 4 290 g 92 469 mmol activated carbon darco g 60 44 g acetone 4305 ml and water 870 ml dl the mixture was heated to reflux 60 64 u00b0 c and held 45 minutes vol 5509 ml the hot slurry was filtered through celite 29 g using isolated vacuum the reactor and filter cake were rinsed with acetone 200 ml and the clear light yellow filtrates were combined the mixture was allowed to cool slowly to 25 u00b0 c over 2 5 hours with stirring to precipitate a fine white solid vol 5665 ml the white slurry was cooled to 0 10 u00b0 c and held for 1 hour the solids were filtered off using isolated vacuum and the liquid level was pulled through the surface of.