ChemicalBook CAS DataBase List Pentamethyldiethylenetriamine

Pentamethyldiethylenetriamine synthesis

6synthesis methods

Product Name:Pentamethyldiethylenetriamine
CAS Number:3030-47-5
Molecular formula:C9H23N3
Molecular Weight:173.3

50-00-0 Synthesis

50-00-0
862 suppliers
$10.00/25g

111-40-0
499 suppliers
$13.44/25ML

3030-47-5
338 suppliers
$5.00/10g

Yield:3030-47-5 85.76 %

Reaction Conditions:

with formic acid in water at 110;Cooling;

Steps:

1.3 (3) Preparation of pentamethyldiethylenetriamine

Add 8.24g (0.08mol) diethylenetriamine in a dry 250mL three-necked flask, place the flask in a cold water bath, add 29.41g (0.64mol) of anhydrous formic acid dropwise, and then add 45.37g 37wt% formaldehyde aqueous solution ( 0.56mol formaldehyde), slowly heat until no large amount of carbon dioxide gas emerges from the flask, then raise the temperature to the temperature of the reaction liquid at about 110°C, and reflux for 12 hours. Then 20 mL of concentrated hydrochloric acid was added. Desolvation and washing with anhydrous methanol three times to obtain the crude product pentamethyldiethylenetriamine hydrochloride. Add the crude product into a 250mL single-necked flask, then add 17.38g (0.11mol) of sodium hydroxide and 100mL of methanol, and heat to reflux for 1h. Precipitate, add metallic sodium to rectify, collect fractions at 206-208°C (101.325kPa), and obtain 11.87g of colorless, transparent and slightly viscous pentamethyldiethylenetriamine with a yield of 85.76%.

References:

CN115340476,2022,A Location in patent:Paragraph 0099; 0115-0120

67-56-1 Synthesis