ChemicalBook CAS DataBase List Bis(2-dimethylaminoethyl) ether

Bis(2-dimethylaminoethyl) ether synthesis

13synthesis methods

Product Name:Bis(2-dimethylaminoethyl) ether
CAS Number:3033-62-3
Molecular formula:C8H20N2O
Molecular Weight:160.26

The main methods for the synthesis of Bis(2-dimethylaminoethyl) ether are:
(1) reaction of sodium dimethylaminoethanol and SO3 or chlorosulfonic acid;
(2) Reaction of trimethylamine with dichloroethyl ether or dimethylaminoethoxyethyl ether;
(3) One-step synthesis of dimethylamine and monoethyleneglycol under solid catalyst.

1704-62-7 Synthesis

1704-62-7
200 suppliers
$6.00/10g

75-50-3
252 suppliers
$15.00/25ml

3033-62-3
298 suppliers
$14.00/1mL

Yield:3033-62-3 132 g

Reaction Conditions:

Stage #1: 1-O-Dimethylaminoethyl-ethylenglykolwith thionyl chloride in toluene; for 1.5 h;Reflux;
Stage #2: trimethylamine at 50 - 80; for 3 h;
Stage #3: with ethylenediamine at 100 - 170; for 3 h;Autoclave;Temperature;

Steps:

8

In a dry 1000ml four-necked flask was added 131g (1.10mol) thionyl chloride and 500g of toluene, cooled to below 20 ° C, dimethylaminoethoxyethanol 133g (lmol) was slowly added dropwise after the end of incubation was incubated Half an hour, and gradually warmed to reflux temperature, reflux incubated for 1 hour, evaporated toluene, cooled to below 50 ° C, 30% trimethylamine 492g (2.5mol), 50 ° C reaction 2 hours, 80 ° C Reaction 1 Hour, the water evaporated to dryness, add ethylenediamine 240g (4.0mol) below 100 ° C, the material was transferred to a 500ml autoclave, warmed to 170 ° C, the reaction for 3 hours, cooled below 20 ° C discharge and Immediately filtered, rinsed with a small amount of ethylenediamine cake, the filtrate distilled after distillation of methylethylenediamine, at 10mmHg column collected 90-110 ° C fraction, 132g, 99.2% by gas chromatography.

References:

CN107286029,2017,A Location in patent:Paragraph 0013