A kind of method for preparing celecipa intermediate compound with high yield under mild conditions
A technique for the production of selexipa and compounds, which is applied in the field of high-yield preparation of selasipa intermediate compounds, and can solve the problem of low activity of 5-chloro-2,3-diphenylpyrazine, diphenyl ethanedione High operational requirements, no industrial value, etc., to achieve the effect of improving production safety, low cost, and easy operation
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Embodiment 1
[0054] Example 1: Preparation of 2-(N-isopropyl-N-4-(hydroxy)butyl)amino-5,6-diphenylpyrazine (II)
[0055] In the 500 milliliter four-necked flask that is connected with stirring, thermometer and condenser tube, add 120 grams of dichloromethane, 21.0 grams (0.1 moles) of benzoin alcohol, 25.0 grams (0.12 moles) of 40% hydrobromic acid, 20~25 ℃ The reaction was stirred for 4 hours to obtain 1,2-diphenyl-2-bromoethanone solution. After the reaction was completed, the layers were separated, and the aqueous layer was extracted twice with dichloromethane (10 grams each time), and the organic phases were combined. The obtained organic phase was transferred to a constant pressure dropping funnel for use. In another 500 ml four-neck flask with stirring, thermometer and condenser tube, add 30 g of dichloromethane, 20 g (0.11 moles) of N-aminoacetyl-N-isopropyl n-butanol, 15.0 g of carbonic acid Potassium, between 30-35°C, add dropwise the solution in the constant-pressure dropping fu...
Embodiment 2
[0057] Example 2: Preparation of 2-(N-isopropyl-N-4-(hydroxy)butyl)amino-5,6-diphenylpyrazine (II)
[0058] In the 500 milliliter four-necked flask that is connected with stirring, thermometer and condenser, add 120 grams of chloroform, 21.0 grams (0.1 moles) of benzoin alcohol, 15.6 grams (0.15 moles) of 35% hydrochloric acid, 30~35 ℃ of stirring reaction 3.5 hours , to obtain 1,2-diphenyl-2-chloroethanone solution, after the reaction was completed, the layers were separated, the aqueous layer was extracted twice with chloroform (10 grams each time), the organic phases were combined, and the resulting organic phase was transferred to a constant In the pressure dropping funnel, ready for use. In another 500 ml four-neck flask with stirring, thermometer and condenser, add 30 gram chloroform, 20 gram (0.11 mole) N-aminoacetyl-N-isopropyl n-butanol, 12.0 gram sodium carbonate, Between 30 and 35°C, add the solution in the constant pressure dropping funnel dropwise for about 1 hou...
Embodiment 3
[0059] Example 3: Preparation of 2-(N-isopropyl-N-4-(hydroxy)butyl)amino-5,6-diphenylpyrazine (II)
[0060] In the 500 milliliter four-necked flask that is connected with stirring, thermometer and condenser, add 120 grams of dichloromethane, 21.0 grams (0.1 moles) of benzoin alcohol, 38.5 grams (0.12 moles) of 40% hydroiodic acid, stir at 20~25 ℃ Reacted for 3 hours to obtain 1,2-diphenyl-2-iodoethanone solution. After the reaction was completed, the layers were separated, the aqueous layer was extracted twice with dichloromethane (10 grams each time), the organic phases were combined, and the resulting The organic phase was transferred to a constant pressure dropping funnel for use. In another 500 ml four-neck flask with stirring, thermometer and condenser tube, add 30 g of dichloromethane, 20 g (0.11 moles) of N-aminoacetyl-N-isopropyl n-butanol, 15.0 g of carbonic acid Potassium, between 30-35°C, add dropwise the solution in the constant-pressure dropping funnel, and drop ...
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