cublium
(Stranger) 05-24-03 14:47 No 435161 |
Cub's having problems with Al/Hg | Bookmark | ||||||
100 grams of ketone was aminated with 25% w/w yield.Cub has used Al/Hg in past with success but this time it was complete failure.Cub followed Os/BB writeup.When methylamine freebase solution was added to rx mix,almost violent reaction kicked in and aluminium started bubbling very fast,some bubbles were even 0,5 cm in diameter.Cub didn't know what to think and added ketone.This didn't slow the reaction and bubbling down as usually,no-no,bubbling increased along with temperature and pretty fast.Rx mix had to be constantly cooled.In an hour reaction was completed.A/B'd,titrated and evapped to get 25,5 grams of white powder as usual but in low yields.Any advice is really appriciated. |
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cublium (Stranger) 05-24-03 19:44 No 435205 |
details | Bookmark | ||||||
Same ketone was used last week with 70 % w/w yields and methylamine is same too.Aluminum used was same as last week,0,1 mm thick.Raf also noticed that during reduction aluminium was covered with some hydroxide and very little shiny alu was seen,usually it doesn't get coated with that hydroxide layer.BTW bioassay proved extremely positive,150 mg and 160 pounds of bodyweight. |
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