Preparation method for 3-piperidyl acrylate
A technology of dimethylaminoacrylate and acrylate, which is applied in the field of industrial synthesis of piperidinyl derivatives, can solve the problems of being too expensive, not suitable for large-scale production, economical and industrializable methods are not common, etc. , to achieve high reaction yield, suitable for industrial production, and low production cost
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0034] The preparation method of the 3-piperidinyl-ethyl acrylate of the present embodiment comprises the following steps:
[0035] In a reaction flask equipped with a reflux condenser and a hydrochloric acid absorption dimethylamine device, add 100g (0.698mol) of N,N-ethyl dimethacrylate, 300ml of toluene, 89g (1.047mol) of piperidine and 2g acetic acid, then stirred and heated to reflux, reflux for 6 hours, gas chromatography GC detected that the raw materials were almost completely converted, the reaction released dimethylamine, absorbed with hydrochloric acid aqueous solution, concentrated under reduced pressure to recover toluene and piperidine after the reaction was completed. The yield of the product was 130.8 g, and the yield was 99.0%. The internal standard content is 97.3%. The internal standard content refers to the amount of 3-piperidyl-ethyl acrylate in the product of this embodiment detected by gas chromatography GC and the amount of 3-piperidyl-ethyl acrylate in...
Embodiment 2
[0039] The preparation method of the 3-piperidinyl-ethyl acrylate of the present embodiment comprises the following steps:
[0040] In a reaction flask equipped with a reflux condenser and a hydrochloric acid absorption dimethylamine device, add 100 g (0.698 mol) of N,N-ethyl methacrylate, 300 ml of toluene, 70 g (0.823 mol) of piperidine and 1.8 G concentration is 98% formic acid, then stir and heat up to reflux, and reflux for 6 hours. GC detects that the raw material is almost completely converted, and the reaction releases dimethylamine, which is absorbed by aqueous hydrochloric acid. After the reaction is completed, concentrate under reduced pressure to recover toluene and piperidine . The yield of the product was 130.2 g, the yield was 98.6%, and the internal standard content was 97.1%.
Embodiment 3
[0042] The preparation method of the 3-piperidinyl-ethyl acrylate of the present embodiment comprises the following steps:
[0043] Add 100g (0.698mol) of N,N-ethyl methacrylate, 300ml of toluene, 100g (1.176mol) of piperidine and 2.5 g of methanesulfonic acid, then stirred and heated to reflux, and refluxed for 6 hours. GC detected that the raw materials were almost completely converted, and the reaction released dimethylamine, which was absorbed with aqueous hydrochloric acid. After the reaction was completed, concentrated under reduced pressure to recover toluene and piperidine. The yield of the product was 130.5 g, the yield was 98.9%, and the internal standard content was 97.5%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More