Method for preparing agomelatine acetyl diamine
A technology of agomelatine acetyldiamine and acetonitrile, applied in the field of medicine, can solve the problems of low yield, complicated operation method of agomelatine acetyldiamine, etc., and achieves high purity, high yield and good preparation method Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0027] First add 100mL of acetic acid to a 500mL autoclave, then carefully add 5g of anhydrous Raney nickel catalyst, 15g of (7-methoxy-1-naphthyl) acetonitrile, 23g of acetic anhydride, anhydrous Raney nickel catalyst and (7-methoxy The mass ratio of base-1-naphthyl) acetonitrile is 0.3:1, and the mol ratio of (7-methoxy-1-naphthyl) acetonitrile and acetic anhydride is 1:3, mixes and obtains reaction solution, then in the reactor Feed hydrogen, and the pressure in the autoclave after completion is 2MPa. Heat the autoclave to 45°C, react for 25 hours, then filter, and concentrate the filtrate under reduced pressure. After concentration, the residue is obtained. Add 100 mL of ethyl acetate to the residue, then stir and wash the residue with 1 mol / L hydrochloric acid, and then Wash the residual solution with saturated sodium chloride solution, dry over anhydrous sodium sulfate, and concentrate under reduced pressure to obtain the residue; then add 20 mL of ethyl acetate to the r...
Embodiment 2
[0031] First add 150mL of acetic acid to a 500mL autoclave, then carefully add 10g of anhydrous Raney nickel catalyst (the mass ratio to (7-methoxy-1-naphthyl)acetonitrile is 0.3:1), 0.15mol (7-methoxy Base-1-naphthyl) acetonitrile (i.e. 30g), 0.45mol acetic anhydride (i.e. 46g), the molar ratio of (7-methoxyl-1-naphthyl) acetonitrile and acetic anhydride used is 1:3, mix Obtain the reaction solution, then feed hydrogen into the reactor, and the pressure in the autoclave after completion is 2MPa. Heat the autoclave to 45°C, react for 25 hours, then filter, and concentrate the filtrate under reduced pressure. After concentration, the residue is obtained. Add 200 mL of ethyl acetate to the residue, and then stir and wash the residue with 1 mol / L hydrochloric acid. Then wash the residual solution with saturated sodium chloride solution, dry over anhydrous sodium sulfate, and concentrate under reduced pressure to obtain the residue; then add 40 mL of ethyl acetate to the residue f...
Embodiment 3
[0033] First add 80mL tetrahydrofuran to a 500mL autoclave, then carefully add 2g of anhydrous Raney nickel catalyst (the mass ratio to (7-methoxy-1-naphthyl)acetonitrile is 0.2:1), 0.05mol (7-methoxy Base-1-naphthyl) acetonitrile (i.e. 10g), 0.1mol acetic anhydride (i.e. 10.2g), the molar ratio of (7-methoxyl-1-naphthyl) acetonitrile and acetic anhydride used is 1:2, Mix to obtain the reaction liquid, then feed hydrogen into the reactor, and the pressure in the autoclave after completion is 3MPa. Heat the autoclave to 50°C, react for 24 hours, then filter, and concentrate the filtrate under reduced pressure. After concentration, the residual liquid is obtained. Add 80 mL of ethyl acetate to the residual liquid, and then stir and wash the residual liquid with 1 mol / L hydrochloric acid. The residue was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain the residue; then 15 mL of ethyl acetate wa...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More