10-04-03 18:58
No 462569
Following the procedure ala Barium's 2c-h chlorination using oxone the following was performed : (copy pasting some from Barium's post here)
1 g 2C-H*HCl (4,6 mmol)
1,4 g Oxone (2,3 mmol)
10 ml MeOH
5 ml water
2C-H*HCl was dissolved in the mixture of water and MeOH in a 100 ml rb flask (at weather temperature 18 deg Celcius) equipped with a magnetic stirbar and the oxone added in three portions during 10 minutes. The cloudy white solution gradually became more cloudy whiteish yellow during 15 minutes. Temperature was not recorded. After 1 hour 20 ml HOAc was added and stirred for 5 more minutes. Initial there was a cloudy yellow liquid.
Now here is where the problems started, half of the solution was put into a sep funnel, there was added 20 ml DCM to the solution and crystals formed falling down to the lower layer, the layer was removed and another 15 ml DCM was added to the solution causing more crystals to fall out. Also none of the yellow color went into the DCM layer.
Both DCM washes and the solution where added together and gravity filtered, the small ammount of white crystals where recovered from the filter.
Looking at the other half of the yellow solution a lot of crystals had formed, the crystals where filtered off.
Now the weird thing is that after the gravity filtration of the first solution (the yellow liquid + DCM) is that while putting the solution back into the sep funnel and letting things to settle no visible layers formed.
The DCM was stripped off under the rotovap, here i made the stupid mistake to heat things over 70 celcius so the oxone started to decompose and everything became a nice black goo liquid the same that happened with my initial 2c-b/oxone tryouts.
Now the funny thing however is that the meltingpoint of the crystals recovered are 218-220 Degree Celcius, has anyone an idea if 2c-c has been formed ?
Perhaps freebasing it should atleast indicate that the crystals are an amine.
Hippler
