Method for preparing ethyl p-methoxy cinnamate
A technology of ethyl cinnamate and p-methoxyl group is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of poor economic benefit and high price
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Embodiment 1
[0012] The preparation method of the solid super base is as follows: add 100g of hydrated alumina dry glue into the flask, open the nitrogen channel and start stirring, slowly heat up to 500°C, keep it for 3h and then cool down to 400°C; add KOH 10g, KNO 3 5g, Na 2 CO 3 7g was stirred and reacted under nitrogen protection for 3h, then 10g of metal sodium was added in batches at the same temperature, and the reaction was continued for 1h and then stopped.
[0013] A kind of method for preparing ethyl p-methoxycinnamate
[0014] Measured 136g of p-methoxybenzaldehyde, 500g of toluene and 10g of solid super base were added to the flask, heated to reflux under stirring, slowly added dropwise a toluene solution (20%) containing 210g of diethyl malonate, and the addition was completed. The reaction was continued at the set temperature for 3 hours, the catalyst was filtered, the toluene was distilled off, and the residue was cooled to slowly separate out 190 g of a pale yellow sol...
Embodiment 2
[0016] The preparation method of the solid super base is as follows: add 100 g of hydrated alumina dry glue into the flask, open the nitrogen passage and start stirring, slowly heat up to 600 ° C, keep it for 3 hours and then cool down to 500 ° C; add KOH 10g, KNO 3 8g, Na 2 CO 3 5g was stirred and reacted under nitrogen protection for 3h, then 13g of metallic sodium was added in batches at the same temperature, and the reaction was continued for 1h and then stopped.
[0017] A kind of method for preparing ethyl p-methoxycinnamate
[0018] Measured 136g of p-methoxybenzaldehyde, 600g of toluene and 15g of solid super base were added to the flask, heated to reflux under stirring, slowly added dropwise a toluene solution (20%) containing 230g of diethyl malonate, and the addition was completed. The reaction was continued at the set temperature for 4 hours, the catalyst was filtered, the toluene was distilled off, and the residue was cooled to slowly separate out 200 g of a pa...
Embodiment 3
[0020] The preparation method of the solid super base is as follows: add 100g of hydrated alumina dry glue into the flask, open the nitrogen passage and start stirring, slowly heat up to 550°C, keep it for 3h and then cool down to 450°C; add KOH 10g, KNO 3 4g, Na 2 CO 3 6g was stirred and reacted under nitrogen protection for 3h, then 12g of metallic sodium was added in batches at the same temperature, and the reaction was continued for 1h and then stopped.
[0021] A kind of method for preparing ethyl p-methoxycinnamate
[0022] Measured 136g of p-methoxybenzaldehyde, 400g of toluene and 18g of solid super base were added to the flask, heated to reflux under stirring, slowly added dropwise a toluene solution (20%) containing 220g of diethyl malonate, and the addition was completed. The reaction was continued at the set temperature for 5 hours, the catalyst was filtered, the toluene was distilled off, and the residue was cooled to slowly separate out 203 g of a pale yellow ...
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