Tetraacetylethylenediamine synthesis
- Product Name:Tetraacetylethylenediamine
- CAS Number:10543-57-4
- Molecular formula:C10H16N2O4
- Molecular Weight:228.24
TAED was prepared by acetylation of diacetylethylenediamine (DAED) with acetic anhydride in a 5 L reactor coupled with a packed distillation column, 2.5 cm in inside diameter and 1 m in length. The reaction temperature was set at 135 °C and the reflux ratio at 6. The molar ratio of acetic anhydride to DAED was varied from 3 to 5. A TAED yield as high as 80% was obtained, higher by 15% than in the absence of distillation.
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Yield:10543-57-4 81.9%
Reaction Conditions:
with solid acid SO4(2-)/Al2O3 at 110 - 160; for 4.5 h;Reagent/catalyst;Temperature;
Steps:
5 Example 5 the preparation of tetracetyl ethylenediamine-4.5hr-catalyst 10wt%
The procedure of Example 3 was repeated, Adding 6.00 g of solid acid SO42- / Al2O3 as catalyst, The remaining composition of the addition ratio and operating conditions to maintain the same, To obtain 77.74 g of product tetraethylethylenediamine, Yield 81.9%. 60.05 g of diacetyl ethylenediamine and 425 g of acetic anhydride were added to a 1 L reaction flask, After heating to reflux at 140 ° C for 2 hours, Start steaming acetic acid for 2.5 hours and control the distillation temperature between 110 ~ 125 , To be cooled cooling crystallization and then filter and dry, 72.31 g of tetraacetylethylenediamine, Yield 76.0%.
References:
China Petroleum Chemical Industry Development co., LTD (TW);CHIANG, PEIYUN;CHEN, CHIHE;HUANG, ZHENWEI TWI527787, 2016, B Location in patent:Page/Page column 11; 12
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