03-22-04 00:27
No 496511
Hi! Two hours ago i started a performic with 130g vacuum refluxed Isosafrole. 40g Na2CO3 or NaHCO3 is needed as buffering complex, i had just crystall soda (Na2CO3.10H2O) in stock, so i heated the so called Crystall Soda (Na2CO3.10H2O) in the oven at 180C for 15mins to remove the water and grinded it (100g gave 40g dry soda). The problem is that this powder does not dissolve in the iso/dcm mix. Should i filter it our and go for some real bakingsoda or will it dissolve after adding the peracid? Thanx.
(Hive Bee)
03-22-04 13:53
No 496613
i filtered it out now and used bakingsoda right from the pharmacy. the solubility is a little bit better, but not as good as i thought. i will add the performicacid now, want to see if this method is really as easy as it seems to be...
(Hive Addict)
03-22-04 14:16
No 496615
it's not supposed to dissolve in DCM, fruitcake!
filter(lambda W : W not in 'ILLITERATE','BULLSHIT')
(Hive Bee)
03-22-04 14:59
No 496620
i like fruits.
thanx for your help, one hour earlier and i could exclude the filtering. but have another question: why doesn't it start to warm up during performic addition? iso/bicarb/dcm mix and performicacid was chilled close to 0 C before addition. thanx
(Hive Addict)
03-22-04 17:22
No 496638
where does it say that you should chill it to 0°C?
why don't you just follow the procedure as it is written?
remove any ice bath and let it run at RT. the DCM does the
temperature regulation. some people even heat to reflux.
filter(lambda W : W not in 'ILLITERATE','BULLSHIT')
(Hive Bee)
03-22-04 23:16
No 496697
i think i misinterpreted LapTop's recipe. i have read a post where one told to cool everything, to prevent boiling. now i see in LabTop's recipe, he is just cooling the formicacid, not everything. after applying some heat to warm it to roomtemp, everything is working like he says. i think i must read more posts and more carefully. thanx for your help.
