I would like to inquire about the use of Formic acid, must I use formic acid 85% or formic acid 94%?

[bitcoinup2020]

Hello
I would like to ask for help from someone who knows.
1. Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
2. The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.

From step 1 and 2, use formic acid 85% or formic acid 94%.

Now I have Formic acid 94% can it be used for both step 1 and 2?

and Method 2
The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.

Do I need to drop 1 drop of formic acid at a time per 1 second from the Dropping funnel while refluxed at 150-170 °C for 7 h?

Please can you explain step 2 to me, thank you very much.

Please tell me, I still don't quite understand this step.

thank you very much

I LOVE BB

 

[w2x3f5]

Are you sure your ketone won't break down?
Where does the temperature of 170 degrees come from?
I don't see the water separation nozzle (Dean-Stark nozzle).
It is very important to use the correct temperature, reaction time and the correct proportion of formamide/meric acid/ketone. Also, hydrolysis is a separate snag.

It is easier for you to make a synthesis from ketone, methylamine and sodium borohydride, or on amalgam. It's easier, faster and the yield will be better.

 

[UWe9o12jkied91d]

As far as I know leuckart with formamide is high yielding

 

[w2x3f5]

Borohydride can give 90 percent of the yield of the substance.
The usual Leuckart-Wallach will give 50-60 percent, if the alkaline hydrolysis is more than 60 percent. If you use the full synthesis modification, you can get 90 percent, but this works for regular P2P.
Here the reaction of a very gentle mdp2p and n-methylformamide, there will be a lot of pitfalls. The borohydride will work better, cleaner, and in higher yields.

 

[bitcoinup2020]

Hi w2x3f5

I don't have a reactor, what device do I use to control the cooling?

 

[bitcoinup2020]

Can you guide me for making the Make MeNH2-gas?
and the use of a MeNH2-gas delivery device. I have Methylamine and Sodium borohydride (NaBH4).

 

[w2x3f5]

Ice bath

 

[bitcoinup2020]

ขอบคุณมากสำหรับคำตอบ

 

[bitcoinup2020]

Thank you very much for the answer.

 

[bitcoinup2020]

Can you guide me for making the Make MeNH2-gas?
and the use of a MeNH2-gas delivery device. I have Methylamine and Sodium borohydride (NaBH4).

 

[w2x3f5]

The forum has all the information, see the topics.