3cmc crystallisation brown paste

[Krimson]

Hello. New to the forum here, actually completely new to this side of the internet in general. It's nice to see the conversations here are quite civil. The info and knowledge of a lot of participants are mind-blowing. For sure the answer to my question already is been written somewhere here but i ain't able to filter it out.

I have 3cmc base oil, dark red color. Really nice fully homogeneous state.
Little smoke was coming of and smelling a bit of mono at the time i started crystallization. Researching here this is cause ain't washed proper enough? Anyway I thought it was ready to proceed so i did.

took 200ml base and 100 ml acetone. Used HCL. ph 6.
I could see reaction starting. After about 15 minutes roomtemp 20c it layered in a light brown solution down and a very little layer dark brown on top.

I stirred it again and I put it in the freezer over night. I Got a very hard dark brown paste in the middle and light brown thick paste around it. Washing it should give me powder no?

I need crystals. I don't think that's happening from out the current status of the product. The positive already anyway is that it brought me here on this site. If anybody also can help me with tips to change or the way from here i would be very happy.

grtzzzz

 

[G.Patton]

Hello and welcome here!
I assume that it has to be a colorless liquid or a little yellowish but not red one. Probably, there are a lot of side products which interfere to crystallize it.
I don't know how did you do this addition exactly, but recommend you dissolve HCl 35% in acetone 1:1 and add dropwise to free base with constant stirring. It's very important to avoid overheating and graduate acidification.
You can try to wash it and recrystallize it again to get a powder.

 

[Krimson]

Thanks for your Reaction. It is much appreciated!

The precursor is also red colored Liquid. Could this be the reason for the red Color? I get the base light red maximum. washed it with distilled water with a little baking soda. Washing it more ain't doing the base any good. Gonna acid later this week. Let you know the result. I use HCL Gas for the acidification. Which ph you recommend?

 

[Yogi]

That's not what i like to hear. It's cas no 34911-51-8. Label reads 3-Chlorophenyl-1Bromoethyl-Ketone. I was told this should be good. synthesis mono on water double amount and p-toluenesulfonic acid as katalyst. Suggestions?

 

[Krimson]

That's not what i like to hear. It's cas no 34911-51-8. Label reads 3-Chlorophenyl-1Bromoethyl-Ketone. I was told this should be good. synthesis mono on water double amount and p-toluenesulfonic acid as katalyst. Suggestions?

 

[William D.]

pH ~ 4.5 for HCl. I think PTSA is used not as a catalyst, but to acidify and obtain the desired form of crystals.