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?
.
 

G.Patton

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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.
 

Jackson

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I saw this guide but its for large scale
 

G.Patton

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What a problem to scale it down proportionately?
 

The-Hive

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It’s normally x10 so iam guessing -10
 

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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Yes, 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
is this right?
 

w2x3f5

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I 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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Sodium 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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