William Dampier gave me the following 4MMC synthesis. We were chatting to and from but since Friday h hasn4 popped over wh9ch is unlike hi. gone and I haven't been able to ask for his advice / help because I feel something is not right in what I'm doing. the ingredients and method are stated below. iI get to the stage where I add equal deionized to the DCM and then i added acid until 5ph,, NEXT BIT I WASNT SURE SO I CHECKED THE PH LEVEL OF TOP LEVE AFYER ADDING ACID AND SHAKE WELL THEN DO PH CHECK ON THE WATER ONLY? ALSO WHEN I AM ADDING THE ACID AND IT GETS TO 5PH DO I CONTINUE TO SHAKE THE ECM, 4MMC AND DEIRONISED
I WAS TOLD AHEN THE PH REACHES 5PH THE 4MMC WILL GET KICKED OJT OF THE DCM AND INTO THE WATER but I'm not sure of it is or not
IM WAITING FOR THE "4mmc WAYER TO CRYSTALISE AT THE MOMENT but I DONT KNOW IF THERE IS ANY 4MMC IN THE WATER for me to. Crystallise, I'm unsure whT fo do
IHAVE I MISSED A SREP iMAYBR?
INGREDIENTS AND METHOD AS GIVEN BY William DAMPIER IS THEY stage missing such as shak
William Dampier gave me the following 4MMC synthesis. We were chatting to and from but he was gone and I haven't been able to ask for his advice / hee the bottle for a set a.oj y of 4m.e
William Dampier method:
1. Add 50g100g200g of BK to the flask (BK - solid substance. You need to work with this with gloves. Use a funnel for a flask. Until the next steps, it would not be bad to get a photo of BK in a flask 2. Add dichlormethane (150mL300mL600mL min) and mix until the entire BK dissolves. Can help dissolve by heating the flask. For heating, we use a container with hot water, heating mantle for flask or a magnetic stirrer hotplate. Mix shaking the flask manually, or with stirring with over-head stirrer or magnetic stirrer. Do not heat mixture higher 40*C 3. When everything is dissolved, add 100mL200mL400mL of aqueous methylamine. It is a stinking poisonous gas in the water that smells like rotten fish. You can easily understand it by its smell, but I do not advise you to inhale it. You can check with indicator paper, it will be alkaline. Add methylamine slowly to avoid overheating. 4. When all the methylamine has been added, heat the mixture to 35-40*C. If the mixture is already at such a temperature, then simply maintain it. A total of methylamine addition, mixing with heating should take 3 hours. After this time, pour in clean water, and separate it from the dichloromethane layer. If the dichloromethane layer smells like rotten fish, repeat the rinse with clean water. 5. Next we will do acidification, there are several routes. For promotion, I will recommend one of my favorite routes. It takes longer but gives good results. We need clean water and glassware for crystallization. Add clean water to the washed layer of dichloromethane (not more than the same amount as the amount of dichloromethane itself) and with good stirring, add hydrochloric acid until pH = 5. After that, we separate the aqueous layer into a glass dish so that its thickness is 1-1.5cm. We leave it at room temperature in a dark place, without a lid. No need to stir. DCM put in the freezer. Expect crystallization
I WAS TOLD AHEN THE PH REACHES 5PH THE 4MMC WILL GET KICKED OJT OF THE DCM AND INTO THE WATER but I'm not sure of it is or not
IM WAITING FOR THE "4mmc WAYER TO CRYSTALISE AT THE MOMENT but I DONT KNOW IF THERE IS ANY 4MMC IN THE WATER for me to. Crystallise, I'm unsure whT fo do
IHAVE I MISSED A SREP iMAYBR?
INGREDIENTS AND METHOD AS GIVEN BY William DAMPIER IS THEY stage missing such as shak
William Dampier gave me the following 4MMC synthesis. We were chatting to and from but he was gone and I haven't been able to ask for his advice / hee the bottle for a set a.oj y of 4m.e
William Dampier method:
1. Add 50g100g200g of BK to the flask (BK - solid substance. You need to work with this with gloves. Use a funnel for a flask. Until the next steps, it would not be bad to get a photo of BK in a flask 2. Add dichlormethane (150mL300mL600mL min) and mix until the entire BK dissolves. Can help dissolve by heating the flask. For heating, we use a container with hot water, heating mantle for flask or a magnetic stirrer hotplate. Mix shaking the flask manually, or with stirring with over-head stirrer or magnetic stirrer. Do not heat mixture higher 40*C 3. When everything is dissolved, add 100mL200mL400mL of aqueous methylamine. It is a stinking poisonous gas in the water that smells like rotten fish. You can easily understand it by its smell, but I do not advise you to inhale it. You can check with indicator paper, it will be alkaline. Add methylamine slowly to avoid overheating. 4. When all the methylamine has been added, heat the mixture to 35-40*C. If the mixture is already at such a temperature, then simply maintain it. A total of methylamine addition, mixing with heating should take 3 hours. After this time, pour in clean water, and separate it from the dichloromethane layer. If the dichloromethane layer smells like rotten fish, repeat the rinse with clean water. 5. Next we will do acidification, there are several routes. For promotion, I will recommend one of my favorite routes. It takes longer but gives good results. We need clean water and glassware for crystallization. Add clean water to the washed layer of dichloromethane (not more than the same amount as the amount of dichloromethane itself) and with good stirring, add hydrochloric acid until pH = 5. After that, we separate the aqueous layer into a glass dish so that its thickness is 1-1.5cm. We leave it at room temperature in a dark place, without a lid. No need to stir. DCM put in the freezer. Expect crystallization
