1) You don't have to add ALL of your nitro before you start add the ketone to get good results.
2) Visually determined by reflux.
3) I dont think it will "hurt" yield, although it may make the workup more difficult, ie emulsions. The amount of base needed will be determined by how much product you actually made. If you only need half did you only yield half??
4) Suggestion, add half the nitro, then add your ketone, and have the drip completed in 30 minutes. Adding the water may help, but in that much excess.. I dunno. Sometimes after washing a rb after a rxn, I just leave the few drops of water in there and call it 5ml's.
What exactly are your yields!? The more info you provide, the more you can be helped.
>>One last observation: reactions using Hg Chloride/Methanol mixed up the day
>>before as opposed to right before use, took much longer for the amalgamation
>>to start (30+ minutes)and did not run as well.
huh? 30+ minutes is long??
Are you ending up with a lot of foil left over after the rxn?