downwardsfromzero wrote:
Without further details of both the entire extraction procedure and the conversion process it's not really that meaningful to speculate.
Thanks for the reply
12hr acid boils on 500g ACRB > reduced > basify with sodium hydroxide > pull with 800mL Xylene in 2 separate jars (400 each jar), whole mix is double boiled whole time. Xylene is so effective historically if hot in pulling damn near everything out with one pull if you use a fair deal for the pull. Tried second pulls many times, nothing came of it when using this much hot Xylene.
800mL total Xylene was defatted (mini-A/B) once, and only once, with 150mL vinegar mixed with 300mL water. That acidic water was then basified again, and pulled with just 500mL Xylene this time. Used FASA on this Xylene and it resulted in probably a total of 13g of fumarates.
Freebased by dissolving all the dried, (acetone washed) fumarates (13g) in minimal near-boiling water, then added sodium carbonate saturated water. About 4g of freebase goo floated to the top and the reaction was done in a few mins.
This end product is really, really oily I notice, and it's kindof a (light) tan color. Am I not doing nearly a thorough enough job defatting? Is it the case that even with perfect defatting, NMT can still make the end product refuse to crystallize no matter what? Thanks again for the help!
EDIT: Also, if it's sodium fumarate, any clue why that would be in my fumarates? Never heard of anyone with this issue