2,2'-oxybis(n,n-diethylethanaMine) synthesis
- Product Name:2,2'-oxybis(n,n-diethylethanaMine)
- CAS Number:3030-43-1
- Molecular formula:C12H28N2O
- Molecular Weight:216.36
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Yield:3030-43-1 95.3%
Reaction Conditions:
with sodium ethanolate in dibutyl ether at 50; for 7 h;
Steps:
2.1 Preparation of bis (2-Diethylaminoethyl) Ether
j0044] Example 2: a bis (2-diethylaminoethyl) ether synthesizing method using N,N-diethylethanolamine, diethylamine and ethyne as raw materials (original raw materials) is performed by the following steps in proper order:10045] step 1: synthesizing:10046] wherein at a room temperature, 117 g N,N-diethylethanolamine (1.0 mol), 268 g diisobutyl ether (as a solvent) and 3.6 g sodium ethoxide are added in a high-pressure reaction dave with a mixing and temperature-measuring device; the dave cover is put on and leakage is inspected; then 6.5 g ethyne (0.25 mol) and 55.0 g diethylamine (0.75 mol) are forced into the dave in proper order; afier feeding, a temperature is raised to 50° C., and kept on for 7 h before completing the reaction;10047] afier reaction, the dave is opened and a filtrate is obtained by filtering the reaction mixture; and step 2:10048] distilling the filtrate obtained at 60° C. and atmospheric pressure for half an hour for the unreacted diethylamine to come out; then proceeding to rectification at reduced pressure intermittently; at a pressure of 1 kPa, collecting the previous fractions (all fractions before 91° C.)- unreacted N,N-diethylethanolamine and solvent; then collecting the fractions at 9 1-93° C. and obtaining bis (2-diethylaminoethyl) etherweighing 51.5 g; wherein a product purity is 99.1%; by taking the consumed ethyne as reference, a yield rate is 95.3%.
References:
US2015/291506,2015,A1 Location in patent:Paragraph 0044; 0045; 0046; 0047; 0048
