Method for synthesizing 4-(dicyanomethylene)-2-tert-butyl-6-(1,1,7,7-tetramethyljulolidin-4-yl-vinyl)-4H-pyran
A technology of tetramethyljulolidine and dinitrile methylene, applied in the field of synthesis of -4-dinitrile methylene-2-tert-butyl-6-pyran, which can solve the problems of long reaction time , to achieve good purity and shorten the purification cycle
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0020] The present invention is implemented according to the following synthetic route:
[0021]
[0022] In a 100ml round bottom flask equipped with an air condenser, add 2.14g (0.01mol) of 2-methyl-6-tert-butyl-4-dicyanomethyl-4H-pyran, 9-formyl-1 , 1,7,7-Tetramethyljulonidine 2.57g (0.01mol), glycerol 55ml (1.0mol), piperidine 3.0ml (0.03mol), after mixing it uniformly at room temperature, add to In a microwave reactor, heated to reflux for 2 minutes, TLC detects that the reaction is complete, the reaction is stopped, the reaction solution is cooled to room temperature, filtered, the filter cake is washed with 30 ml of absolute ethanol, repeated 3 times, and the filter cake is dried to obtain (E)-4-Dinitrile methylene-2-tert-butyl-6-(1,1,7,7-tetramethyljulonidine vinyl)pyran. Then the vacuum degree is 1.0×10 -3 pa, temperature is 220°C, after sublimation purification, 3.85 g of red solid is obtained, with a yield of 85% and a purity of 99.6%.
[0023] Melting point: 299.8-300....
Embodiment 2
[0027] In a 100ml round bottom flask equipped with an air condenser, add 2.14g (0.01mol) of 2-methyl-6-tert-butyl-4-dicyanomethyl-4H-pyran, 9-formyl-1 , 1,7,7-Tetramethyljulonidine 3.86g (0.015mol), glycerol 66ml (1.2mol), piperidine 3.0ml (0.03mol), after mixing it uniformly at room temperature, add it to In a microwave reactor, heated to reflux for 2 minutes, TLC detects that the reaction is complete, the reaction is stopped, the reaction solution is cooled to room temperature, filtered, the filter cake is washed with 30 ml of absolute ethanol, repeated 3 times, and the filter cake is dried to obtain (E)-4-Dinitrile methylene-2-tert-butyl-6-(1,1,7,7-tetramethyljulonidine vinyl)pyran. Then the vacuum degree is 1.0×10 -3 pa, temperature is 220°C, after sublimation purification, 3.86 g of red solid is obtained, with a yield of 85.2% and a purity of 99.6%.
Embodiment 3
[0029] In a 100ml round bottom flask equipped with an air condenser, add 3.21g (0.015mol) of 2-methyl-6-tert-butyl-4-dicyanomethyl-4H-pyran, 9-formyl-1 , 1,7,7-Tetramethyljulonidine 2.57g (0.01mol), glycerol 55ml (1.0mol), piperidine 5.0ml (0.05mol), after mixing it uniformly at room temperature, add to In a microwave reactor, heated to reflux for 2 minutes, TLC detects that the reaction is complete, the reaction is stopped, the reaction solution is cooled to room temperature, filtered, the filter cake is washed with 30 ml of absolute ethanol, repeated 3 times, and the filter cake is dried to obtain (E)-4-Dinitrile methylene-2-tert-butyl-6-(1,1,7,7-tetramethyljulonidine vinyl)pyran. Then the vacuum degree is 1.0×10 -3 pa, temperature is 220°C, after sublimation purification, 3.86 g of red solid is obtained, with a yield of 85.2% and a purity of 99.6%.
PUM
| Property | Measurement | Unit |
|---|---|---|
| melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More