2-[2-(Dimethylamino)ethoxy]ethanol synthesis
- Product Name:2-[2-(Dimethylamino)ethoxy]ethanol
- CAS Number:1704-62-7
- Molecular formula:C6H15NO2
- Molecular Weight:133.19
50-00-0
929-06-6
1704-62-7
1. Synthesis step: 63.1 g of diethylene glycolamine (0.6 mol) and 34.5 g of paraformaldehyde (1.2 mol) were added to a 250 mL three-necked flask and stirred for 30 minutes. Subsequently, 63 g of formic acid (1.2 mol, 88%) was added slowly and dropwise. The reaction mixture was heated to 100-110°C and kept at this temperature for 1 hour. Upon completion of the reaction, 30 g of the fraction was distilled under reduced pressure (vacuum -0.094 MPa, kettle temperature 80°C). At this time, the content of the product 2-[2-(dimethylamino)ethoxy]ethanol was 90.0% and the content of impurity (S-2) was 9.8%. 2. Purification step: the above reaction solution was transferred to a 500 mL distillation flask and distilled under reduced pressure (-0.094 MPa). Firstly, the fraction at 62°C was collected, which was mainly n-butanol ester exchange product and butyl formate. Subsequently, the fraction at 121 °C, the target product 2-[2-(dimethylamino)ethoxy]ethanol, was collected, and a total of 128.3 g was obtained in 96.5% yield and 99.9% product purity.
Yield:1704-62-7 96.5%
Reaction Conditions:
Stage #1: formaldehyd;2-(2-Aminoethoxy)ethanol for 0.5 h;
Stage #2: with formic acid at 100 - 110; under 705.071 Torr; for 2 h;
Stage #3: with butan-1-ol at 120; for 4 h;Reagent/catalyst;Temperature;
Steps:
Example 1 A DMAEE synthesis method comprising the steps of: diethylene glycolamine, paraformaldehyde and formic acid as starting materials,
1). Synthesis To a 250 ml three-necked flask were added 63.1 g of diethylene glycol amine (0.6 mol), 34.5 g of paraformaldehyde (1.2 mol), stirred for 30 minutes,63 g of formic acid (1.2 mol, 88%) was added dropwise at a temperature of 100 to 110 ° C, and the reaction was carried out at about 100 ° C for 1 hour. 30 g (vacuum - 0.094 MPa, kettle temperature 80 ° C) was distilled off under reduced pressure. The end of steaming,The product content was 90.0% and the impurity (S-2) content was 9.8%. _: The step 2) of the liquid to transfer to 500 ml distillation flask in the vacuum degree is -0.094 mpa under reduced pressure distillation, 62 °C component is a normal butanol ester exchange down of the formic acid is ding Chunzhi, 121 °C DMAEE component namely the products. Collecting 121 °C component 128.3g, yield 96.5%, content of 99.9%.
References:
CN106748831,2017,A Location in patent:Paragraph 0043-0058; 0064
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![2-[2-[2-(dimethylamino) ethoxy]ethoxy]-ethanol](/CAS/GIF/2741-30-2.gif)
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