01-23-04 00:48
No 484084
hi i have a problem understanding something from MDP2P production using the Spiceboy SRV/KRV found at ../rhodium /wacker.
my problem is in the text it sayes you ad these 1 g PdCl2
6 g CuCl2
250 ml denatured alcohol
50 ml ultra clean, vac distilled safrole in the 2L flask thats a total of 300ml. and you make yuor ketone. now when done it sayes to Hit the stuff with about 200-300 ml of dilute HCl (maybe 0.1M HCL). that gives u a total of 500-600ml in the flask. now the tekst just stopes and sayes The result? 37 ml of ketone from 50 ml safrole.
my question is how do you get that 37ml of ketone from the 500-600ml in the flask.
01-23-04 17:51
(Rated as: redundant)
(Greenhorn)
01-23-04 21:28
No 484237
Silly little bee! You dont know?
After you add your hcl solution to your post wacker contents, Shake it a bit To make sure its mixed. Let it seperate. Add about 100ml of dcm to take up your organic phase.Shake let settle. Us your sep funnel to seperate your dcm from the other stuff. keep the dcm. Repeat again with dcm. This time only use 50ml. Once more with 50ml of dcm. Wash your dcm with baking soda solution and brine solution 3 times each. Distill off dcm. Distill ketone.
I went into the business for the money, and the art grew out of it.-Charlie Chaplin
(Hive Bee)
01-23-04 22:11
No 484243
hehe no i just wasent sure because i stuck to the text completly. just a last thing when adding DCM where does it settle out to the top or bottom.
and when washing the DCM where does it then settle out top or botom of the washes. btw thanks for the help.
(Stranger)
01-24-04 00:12
No 484260
DCM will settle on the bottom of the separatory funnel. Consider its density of 1,3 g/ml and compare it with water (1 g/ml).
I have never performed a wacker oxidation, but it sounds to me it's very aqueous at this point, hence the DCM probably has a higher density than the mixture of compounds in the aqueous solution.
01-24-04 03:31
(Rated as: insignificant)
(Greenhorn)
01-24-04 20:23
No 484403
Your better off trying something else besides the O2 wacker.There are many wackers that will give you your ketone. The O2 wacker is kinda funny and sometimes hard to get to work if not shaken very very hard.
I went into the business for the money, and the art grew out of it.-Charlie Chaplin
(Newbee)
01-24-04 23:47
No 484445
Consider its density of 1,3 g/ml and compare it with water (1 g/ml).
When doing separations, you will rarely find that that your dcm phase will be 1.3 g/ml and your aqueous phase 1.0 g/ml. If you're looking at these specific gravities in a post-reaction work up sense, you must remember that there's gonna be stuff dissolved in both layers, affecting respective densities.
It makes little difference in the case of dcm/water since their densities are considerable different, but it can in other cases.
If you have (for whatever reason) a product in chlorobenzene (sp 1.105) and you wash it with brine (sp 1.230) then the aqueous layer will go to the botton and the np will stay on top, whereas washing with dh20 will result in the opposite.
(Hive Bee)
01-25-04 01:04
No 484459
ok thanks for that tip but in my case it should seperate to the bottom and i intend to wash my dcm with dh2o.
btw i have just distilled some dcm from a paintremover. now i have never seen dcm before it came over at 37c and looks like water clear. thats it when washing my dcm with dh20 how can i se where the layeres are meeting is it hard or easy.
and when i add my 100ml dcm to the wacker content in the flask will it then also settle to the bottom or top.
(Hive Bee)
01-25-04 07:47
No 484487
Have you made ketone before? Have you done the benzo wacker? Take picklers advice on the O2 KRV and hold off until you have some time to play around. Theze days sassy is too valuable to throw haphazardly into a KRV. There are a LOT of factors involved in the writeup that cant really bee described with 100% clarity..especially for a NewBee. If you can get PdCl2 you can get hydroquinone. Hydroquinone + H2O2 + I2 = benzo. Benzo + Sassy = 99.9% ketone success rate. KRV = unknown....
Regarding your DCM it will always be on the bottom. The two layers can be completely clear and you will still see a sep line. Its not about color..its about density.
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(Hive Bee)
01-25-04 14:48
No 484508
thanks for the help. and yes this is my first try of making ketone i have tried to get hold of hydroquinone from the net but its imposible i also tried ordering some hydroquinone from the net from USA but they dont export it to EU so its hard for me to get hold of until i get some i must do it this way. but thanks for the help
.
01-25-04 21:43
(Rated as: offending)
(Hive Bee)
01-25-04 23:24
No 484549
If it was ketone in the first place - then maybe you should distill that black tar shit, the fact that it turned black means that it certainly wasn't pure in the first place. The performic also yields gunkier stuff after basification.