Hello, I'm getting close to changing the solvent I'm currently using. The choice, for known reasons, fell on DCM, no less, looking in the sub-topics from the attached there synthesis on DCM I drew the following proportions:
100g bk4 in 300ml dcm and to this 200ml m40 water solution. The whole heated and stirred 2h at 40 degrees
Well, and I was just about to get down to it but in the topic with the crystallization of 4mmc I found the statements of a certain person who, in my opinion judging by her statements, has a great deal of knowledge in this subject. Collecting information from several of her posts into one comes out something like this:
100g of bk4 in 250ml of DCM, to this 150ml of m40 solution in water where the reaction takes 4h at 32-36 degrees C (at 38 degrees DCM boils and this is to be avoided so that impurities do not form) where half of the m40 is added at the beginning and the other half after 1 hour from the start of the reaction.
And here is my question, is it actually sensible to run the reactions at 5 degrees less but for 2h longer? Will this actually affect the yield significantly and the purity of the resulting product? According to this person, running the synthesis at 32-36 degrees for 4h yields about 670-690g of flour from 1kg of 2b4m, in crystals 640-650g which is an excellent result.
Does anyone have knowledge of the best amount of m40 to add for 1kg of bk4 running the synthesis in DCM for the previously mentioned 40 degrees for 2h and 32-36 degrees for 4h?
Greetings
100g bk4 in 300ml dcm and to this 200ml m40 water solution. The whole heated and stirred 2h at 40 degrees
Well, and I was just about to get down to it but in the topic with the crystallization of 4mmc I found the statements of a certain person who, in my opinion judging by her statements, has a great deal of knowledge in this subject. Collecting information from several of her posts into one comes out something like this:
100g of bk4 in 250ml of DCM, to this 150ml of m40 solution in water where the reaction takes 4h at 32-36 degrees C (at 38 degrees DCM boils and this is to be avoided so that impurities do not form) where half of the m40 is added at the beginning and the other half after 1 hour from the start of the reaction.
And here is my question, is it actually sensible to run the reactions at 5 degrees less but for 2h longer? Will this actually affect the yield significantly and the purity of the resulting product? According to this person, running the synthesis at 32-36 degrees for 4h yields about 670-690g of flour from 1kg of 2b4m, in crystals 640-650g which is an excellent result.
Does anyone have knowledge of the best amount of m40 to add for 1kg of bk4 running the synthesis in DCM for the previously mentioned 40 degrees for 2h and 32-36 degrees for 4h?
Greetings
