New Etofibrate preparation method
A technology based on fibrate and reaction, applied in organic chemistry and other directions, can solve the problems of difficult removal of solvents, high melting point, high toxicity of 2-chloroethanol, etc., and achieve the effect of avoiding difficult removal.
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Embodiment 1
[0024] Add 1 L of toluene to the water separation reaction flask, add 1 mol of p-chlorophenoxyisobutyric acid, 1 mol of 2-bromoethanol, and 0.01 mol of p-toluenesulfonic acid, and heat up and reflux for 12 hours. After the reaction is complete, cool down to room temperature, filter, separate, and remove the solvent to obtain colorless 2-bromoethyl p-chlorophenoxyisobutyrate.
[0025] Add 1 mol of 2-bromoethyl p-chlorophenoxyisobutyrate, 1 mol of nicotinic acid, and 1 L of toluene into the reaction flask, heat and reflux for 8 hours, slowly add 1 mol of triethylamine dropwise during the reaction, after the reaction is completed, extract and keep the organic layer , remove the solvent to get Etofibrate, melting point 50°C~51°C (50°C~51°C in literature), ESI-MS (m / z): 363.8 (M+H + ), elemental analysis (C 18 h 18 ClNO 5 ) found value (theoretical value): C 59.41% (59.43%), H 5.01% (4.99%), N 3.94% (3.95%).
Embodiment 2
[0027] 1 L of xylene was added to the water separation reaction flask, 1 mol of p-chlorophenoxyisobutyric acid, 2 mol of 2-bromoethanol, and 0.01 mol of benzenesulfonic acid were added, and the temperature was raised to reflux for 16 hours. After the reaction is complete, cool down to room temperature, filter, separate, and remove the solvent to obtain colorless 2-bromoethyl p-chlorophenoxyisobutyrate.
[0028] Add 1 mol of 2-bromoethyl p-chlorophenoxyisobutyrate, 1 mol of nicotinic acid, and 1 L of toluene into the reaction flask, heat and reflux for 4 hours, slowly add 1 mol of pyridine dropwise during the reaction, extract after the reaction, keep the organic layer, remove Solvent obtained from Etofibrate, melting point 50°C-51°C (50°C-51°C in literature), ESI-MS (m / z): 363.8 (M+H + ), elemental analysis (C 18 h 18 ClNO 5 ) measured value (theoretical value): C 59.41% (59.43%), H 5.01% (4.99%), N 3.94% (3.95%).
Embodiment 3
[0030] 1 L of xylene was added to the water separation reaction flask, 2 mol of p-chlorophenoxyisobutyric acid, 1 mol of 2-bromoethanol, and 0.01 mol of p-toluenesulfonic acid were added respectively, and the temperature was raised to reflux for 8 hours. After the reaction is complete, cool down to room temperature, filter, separate, and remove the solvent to obtain colorless 2-bromoethyl p-chlorophenoxyisobutyrate.
[0031] Add 1 mol of 2-bromoethyl p-chlorophenoxyisobutyrate, 1 mol of nicotinic acid, and 1 L of toluene into the reaction flask, heat to reflux for 16 hours, slowly add 1 mol of N-methyltetrahydropyrrole in the reaction, and extract after the reaction is completed. Take the organic layer and remove the solvent to obtain etofibrate with a melting point of 50°C to 51°C (50°C to 51°C in literature), ESI-MS (m / z): 363.8 (M+H + ), elemental analysis (C 18 h 18 ClNO 5 ) measured value (theoretical value): C 59.41% (59.43%), H 5.01% (4.99%), N 3.94% (3.95%).
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