N,N-Diisopropylethylamine synthesis
- Product Name:N,N-Diisopropylethylamine
- CAS Number:7087-68-5
- Molecular formula:C8H19N
- Molecular Weight:129.24
1), take paraldehyde as raw material, in solvent, under the temperature of normal pressure and 22 ~ 28 ℃, under the effect of an acidic catalyst, reacted 20 ~ 40 minutes;
2), in the reaction product of step 1) gained, add Diisopropylamine and as the metal hydride of reductive agent, insulation reaction 10 ~ 30 minutes; Get DIPEA;The mol ratio of Diisopropylamine and paraldehyde is 1:0.34 ~ 0.4, and the mol ratio of Diisopropylamine and metal hydride is 1:1 ~ 1.2; The mass ratio of an acidic catalyst and Diisopropylamine is 1% ~ 5%;
3), with step 2) behind the reaction solution of the gained decompression desolvation, regulate pH=13, pass through again separatory rectifying, obtain DIPEA.
Yield:7087-68-5 97.2%
Reaction Conditions:
with potassium hydroxide in butan-1-ol at 115; for 7 h;Solvent;Reagent/catalyst;Temperature;
Steps:
4 Example 4
101.1 g (1.0 mol) of diisopropylamine,249.0 g (1.5 mol) of tetraethylammonium chloride,101.1 g n-butanol,112 g (2.0 mol) of potassium hydroxide was added to a 1000 ml three-necked flask,Heated to reflux,And the reaction was carried out for 7 hours after the reflux temperature (115 ° C)Cooled to room temperature,After the reaction mixture was removed from the rotary evaporator,Washed with 200 mL * 3 of deionized water,Combined to collect three times of washing the oil phase direct atmospheric distillation,Fraction collected 125-127 125.4g,That is the product DIPEA,Yield 97.2%The purity was 99.5% by gas chromatography.
References:
CN106478423,2017,A Location in patent:Paragraph 0018-0038
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