QUESTION about synthesis of 4mmc and 3cmc

Jackson

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Hello. I discovered this wonderfull forum about 2 months ago and its so full of great and usefull information.. it makes me regret I didn't learn chemistry in highschool at least..
I watched all the videos posted here.

I wish to produce at medium scale.

I want to make 4mmc and 3cmc. I understand the procedure is the same the only diference is the precursor you start with?
for 4mmc its 2-bromo-4-methylpropiophenone aka 2b4mp? and for 3cmc is
2-Bromo-3'-chloropropiophenone aka 2b3c
I bought some lab equipment.
I have a overhead mixer, 3000ml beaker and a sepparatory funnel but I can buy something else if it's needed.



The simplest method from my noob point of view is this one:

this method seems easy to make, but this method is from
4'-methylpropiophenone and if I buy
2-bromo-4-methylpropiophenone from the forum I will only need to follow the video from 3:23. right?

after 3:23 he gets "The 4-Methylpropiophenone bromination gives 2-bromo-4-Methylpropiophenone in benzene."
I can`t find benzene but I understand toluene is good also.
so in order to be able to imitate the video I will need to start with toluene and add 2-bromo-4-Methylpropiophenone ? then continue like in the video?

also.. I can't find Hydrochloric Acid HCI but I found HBr Hydrobromic Acid.
so can I use toluene instead of benzene and HBr instead of HCI?
.
 

Jackson

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and if I use toluene instead of benzene what do I need to do different from the video?
because I came across this post where someone mentiones
benzene is carcinogenic record video of 4mmc production using nmp benzene is fun and inefficient 40% of the final product very little per 100g bk4 you need to use a 2l flask I use a 2l glass bottle and it yields 300g and 350g of the final crystal product. If you are using benzene toulen dcm xylene nmp you must use different cooking temperatures and the time is different. I do not use a flask, but an ordinary wine bottle, a bucket, a conical separator for wine, cloth for filtration and a centrifuge for drying clothes.

so the procedure is different if I use different solvent ?

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G.Patton

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I want to make 4mmc and 3cmc. I understand the procedure is the same the only diference is the precursor you start with?
for 4mmc its 2-bromo-4-methylpropiophenone aka 2b4mp? and for 3cmc is
2-Bromo-3'-chloropropiophenone aka 2b3c
JacksonHello, correct
2-bromo-4-methylpropiophenone from the forum I will only need to follow the video from 3:23. right?
No, read carefully
From 6:17 to 9:02

Methylamination reaction. The solution of 2-Bromo-4-Methylpropiophenone in benzene is poured back into the flask, methylamine is poured.

so in order to be able to imitate the video I will need to start with toluene and add 2-bromo-4-Methylpropiophenone ? then continue like in the video?
You shouldn't imitate the video. You have to understand what are you doing and processes there. It take some time but it isn't possible to learn everything for beginner. I strongly recommend you to sink your teeth into every manipulation and step, parse all questions before to start with small scale synthesis.
Read and watch this topic also. If you don't understand smth, google it or look at Lab FAQ section. There are everything you need to know for successful synthesis.
 

Jackson

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Hello, correct

No, read carefully



You shouldn't imitate the video. You have to understand what are you doing and processes there. It take some time but it isn't possible to learn everything for beginner. I strongly recommend you to sink your teeth into every manipulation and step, parse all questions before to start with small scale synthesis.
Read and watch this topic also. If you don't understand smth, google it or look at Lab FAQ section. There are everything you need to know for successful synthesis.
G.PattonI saw this guide but its for large scale
 

Jackson

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yes I wish to start with small scale and after some successful batches I can scale up.. but because I don`t have chemistry bases of knowledge I wish to try making it and I will learn by practice I hope :))
 

The-Hive

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Shake and bake with dcm as a try out id say small scale

@Netflix has a good write up
 

w2x3f5

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Hello. I discovered this wonderfull forum about 2 months ago and its so full of great and usefull information.. it makes me regret I didn't learn chemistry in highschool at least..
I watched all the videos posted here.

I wish to produce at medium scale.

I want to make 4mmc and 3cmc. I understand the procedure is the same the only diference is the precursor you start with?
for 4mmc its 2-bromo-4-methylpropiophenone aka 2b4mp? and for 3cmc is
2-Bromo-3'-chloropropiophenone aka 2b3c
I bought some lab equipment.
I have a overhead mixer, 3000ml beaker and a sepparatory funnel but I can buy something else if it's needed.



The simplest method from my noob point of view is this one:

this method seems easy to make, but this method is from
4'-methylpropiophenone and if I buy
2-bromo-4-methylpropiophenone from the forum I will only need to follow the video from 3:23. right?

after 3:23 he gets "The 4-Methylpropiophenone bromination gives 2-bromo-4-Methylpropiophenone in benzene."
I can`t find benzene but I understand toluene is good also.
so in order to be able to imitate the video I will need to start with toluene and add 2-bromo-4-Methylpropiophenone ? then continue like in the video?

also.. I can't find Hydrochloric Acid HCI but I found HBr Hydrobromic Acid.
so can I use toluene instead of benzene and HBr instead of HCI?
.
JacksonYes, you can use toluene instead of benzene, you can use xylenes. hydrobromic acid gives a specific product, it is slightly different from hydrochloride.
It is important to choose a good time for amination and a good temperature, about 2 hours 30 minutes and about 60 degrees (you cannot heat the reaction directly, it is very advisable to heat it through a water bath).
 

Jackson

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I was told shipping Methylamine was banned in china.. and that I must use
Methylamine hcl

I fount these instructions here on bbgate
Preparation of the maximum pure 40% methylamine solution from methylamine hydrochloride can be carried out as follows:
Materials:
- Methylamine hydrochloride (about 160 g)
- Distilled water (about 240 ml)
- Glass flask with a volume of about 500 ml
- Magnetic stirrer
- Thermometer
- Unloading crane
- Glass pipette
Steps:
1. Prepare 240 ml of distilled water in a glass flask with a volume of about 500 ml.
2. Put methylamine hydrochloride in a flask of water.
3. Place the flask on the magnetic stirrer and start stirring.
4. Preheat the mixture to a temperature of 50-60°C, using a thermometer to control the temperature.
5. Continue heating and stirring until the methylamine hydrochloride is completely dissolved.
6. Bring the volume of the solution to 400 ml, adding distilled water, if necessary.
7. Cool the mixture to room temperature while continuing to stir.
8. Adjust the pH to a value of 10-11 using a 10% NaOH solution.
9. Check the concentration of methylamine in the solution using test strips or another method, and, if necessary, adjust the concentration by adding either water or methylamine hydrochloride.
10. Leave the mixture for a few hours or overnight so that all impurities settle to the bottom of the flask.
11. Filter the solution through a filter to remove any remaining impurities.
12. Ready-made methylamine 40% solution can be used in appropriate applications.
Please note that when using any chemicals, appropriate safety measures must be observed, including but not limited to: work in a well-ventilated area, use protective clothing and gloves.
is this right?
 

w2x3f5

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I was told shipping Methylamine was banned in china.. and that I must use
Methylamine hcl

I fount these instructions here on bbgate

is this right?
JacksonI don’t like the idea of trying to collect methylamine free base in a small volume of hot water, since the mixture contains sodium chloride which will displace methylamine gas. It is better to collect the gas in separate clean water or an organic solvent.
 

Jackson

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WillD

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JacksonSodium hydroxide is needed if you use methylamine hcl. The right amount is approximately 1kg of NaOH per 1kg of BK4 (with a small excess)
 
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