ChemicalBook CAS DataBase List N,N,N',N'-Tetramethylethylenediamine

N,N,N',N'-Tetramethylethylenediamine synthesis

10synthesis methods

Product Name:N,N,N',N'-Tetramethylethylenediamine
CAS Number:110-18-9
Molecular formula:C6H16N2
Molecular Weight:116.2

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Yield:110-18-9 98.6%

Reaction Conditions:

with 1-ethyl-2-pyrrolidinone;sodium stannate(IV) trihydrate;alumina;calcium hydroxide at 45 - 80; for 6 h;Autoclave;Inert atmosphere;Reagent/catalyst;Temperature;

Steps:

1-5 Example 2

Preparation of composite catalyst TZOH: 500g Na2SnO3·3H2O (sodium stannate trihydrate),100gCa(OH)2 (calcium hydroxide) is dissolved in 3600g of deionized water, and the temperature is raised to 60,Add 1000g of γ-alumina and immerse it at 60 for 12h,The filter cake obtained by suction filtration was dried in an oven at 120°C for 12 hours,Finally moved to the muffle furnace, in a nitrogen atmosphere at a temperature of 3 /min to 500 ~ 550 roasting for 8 hours,Then, it is naturally cooled to normal temperature under the protection of nitrogen, and pulverized to prepare the composite catalyst TZOH.Put 500g of N-ethylpyrrolidone and 30g of the prepared composite catalyst TZOH into a 1-liter autoclave,The autoclave is equipped with a stirring temperature measuring device, and then the lid is covered. After nitrogen replacement, 26g acetylene is introduced. After the temperature stabilizes,Then pass in 180g of dimethylamine, the molar ratio of acetylene and dimethylamine is 1:4, and then heat at 45°C for 2 hours.Then it was kept at 80°C for 4 hours.After the reaction, the excess dimethylamine was absorbed and applied with N-methylpyrrolidone, and then the autoclave was relieved to normal pressure.The reaction material is filtered, the catalyst is recovered, the mother liquor is rectified, and the fraction at 118122/760mmHg is collected.114.4g of tetramethylethylenediamine was obtained, the content was 99.3% by gas chromatography, and the yield was 98.6% (calculated as acetylene).The bottom of the kettle is the solvent N-ethylpyrrolidone, 432g, recovery rate: 86.4%.

References:

CN111440075,2020,A Location in patent:Paragraph 0051-0067