N-Methyl-N-(N,N-dimethylaminoethyl)-aminoethanol synthesis

Yield:2212-32-0 95.2%

Reaction Conditions:

Stage #1: formaldehyd;2-(2-Aminoethylamino)ethanol at 80 - 90; for 0.5 h;
Stage #2: with formic acid at 80 - 90; for 2 h;
Stage #3: in butan-1-ol at 120; for 4 h;Temperature;Solvent;

Steps:

1

1), synthesis:To a 500 ml three-necked flask was added 104 g of hydroxyethyl ethylenediamine (1.0 mol), 94.7 g of paraformaldehyde (3 mol, 95%), stirred for 30 minutes, and at room temperature of 80-90 ° C 156.8 g of formic acid (3 mol, ), About 1 hour dropping end, continue to control the temperature of 80-90 ° C for 1 hour. 70g (vacuum-0.094MPa, kettle temperature: 80C) was distilled off under reduced pressure. The product was analyzed by gas chromatography at a concentration of 91.8% and 8% of the impurity S-2 (i.e., by-product N, N, N'-trimethyl-N'-ethylidene-ethylenediamine).
2), transesterification:100 g of n-butanol was added to the three-necked flask of step 1) and the temperature was raised to 120 ° C for 4 hours to effect the reaction of the by-product N, N, N'-trimethyl-N'-ethylidene- Ammonia transesterification reaction to produce TMAEEA, by gas chromatography analysis, impurity S-2 content of 0.05%, after cooling back.
3), distillation purification:The liquid of step 2) was transferred to a 500 ml rectification flask under reduced pressure at a vacuum of -0.094 MPa, a component at 62 ° C was n-butanol and a transesterified n-butanolate, 118 ° C component Ie product TMAEEA. A mixture of 139 g at 118 ° C was collected, the yield was 95.2% and the content was 99.9%.

References:

CN106748826,2017,A Location in patent:Paragraph 0040-0064