07-15-04 20:01
No 519688
Swim dreamed the classic MM Benzo wacker with one twist. Swim messed up and ran the wacker for eight hours at 70c rather than three hours as MM recommended. Swims yield was low at only 50gms. Also Swims X2 distilled saffy is cloudy. It refracts well but really expected it to clear up on second distillation. Can some more experienced bees help swim interpret these strange dreams?
(stranger)
(Stranger)
07-18-04 13:01
No 520133
<<Swim messed up and ran the wacker for eight hours at 70c rather than three hours as MM recommended. Swims yield was low>>
I believe most people run the reaction for 3 hours since it is a rather fast reaction and most of the synthesis occurs at the beginning. Running the reaction longer does no more than cause polymerization of the ketone. I'm guessing that the amount of ketone synthesized after 3hours is much less than the amount polymerized and thus, low yields.
But thats just my amateur mind taking a stab at it.
(Hive Bee)
07-19-04 13:13
No 520318
You are correct in hoping that your saf should be water clear,and P suspects that is where most of your problem lies.As to what the cloudiness is, check what the stuff was stored in.A long time ago,P stored some in a white plastic container (that was not PP or PE) and the plastic got all soft and mushy (just like the top of P's My Weigh scale)and the saf was a cloudy white from dyes or whatever,and was thrown out.
Don't know if you should aminate it though...
P lets his wacks run for 6 hours at 60 C or so and always gets 115 to 120g of very pure double distilled ketone back,from the methylman writeup.Never tried the 3 hour thing.