A kind of fullerene pyrrolidine derivative and preparation method thereof
A technology for fullerene pyrrolidine and derivatives, which is applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, chemical instruments and methods, etc., can solve the problems of poor solubility, unsatisfactory targeting, and limited application.
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Embodiment 1
[0032] The method for preparing 3-(4-nitrophenyl)acrolein described in this embodiment comprises the following steps:
[0033] Get 5.0g (66mmol) of p-nitrobenzaldehyde and 10.0mL of acetaldehyde into the three-necked flask, add 10mL of 20% potassium hydroxide-methanol solution in the dropping funnel, stir magnetically, and cool the reaction with an ice-salt bath bottle, when the temperature drops to 0ˉ5°C, slowly add 5mL potassium hydroxide-methanol solution dropwise under magnetic stirring, react for 40 minutes, then add 5mL potassium hydroxide-methanol solution dropwise, continue to react at about 10°C for 40 minutes, and cool down at 5°C The following reaction mixture is solidified, add 16 mL of acetic anhydride, heat on a water bath for 30 minutes, pour into 120 mL of hot water, add 16 mL of concentrated hydrochloric acid, heat in a water bath for 20 minutes, and let stand for 24 hours. Crystals were precipitated, filtered by suction, washed, and recrystallized in 30% aque...
Embodiment 2
[0040] The method for preparing 3-(4-nitrophenyl)acrolein described in this embodiment comprises the following steps:
[0041] Get 5.0g (66mmol) p-nitrobenzaldehyde and 10.0mL acetaldehyde into the three-necked flask, add 10mL mass fraction of 10% potassium hydroxide-methanol solution in the dropping funnel, stir magnetically, and cool the reaction with an ice-salt bath bottle, when the temperature drops to 0ˉ5°C, slowly add 5mL potassium hydroxide-methanol solution dropwise under magnetic stirring, react for 40 minutes, then add 5mL potassium hydroxide-methanol solution dropwise, continue to react at about 10°C for 40 minutes, and cool down at 5°C The following reaction mixture is solidified, add 16 mL of acetic anhydride, heat on a water bath for 30 minutes, pour into 120 mL of hot water, add 16 mL of concentrated hydrochloric acid, heat in a water bath for 20 minutes, and let stand for 24 hours. Crystals were precipitated, suction filtered, washed, and recrystallized in 30%...
Embodiment 3
[0043] The method for preparing 3-(4-nitrophenyl)acrolein described in this embodiment comprises the following steps:
[0044] Get 5.0g (66mmol) of p-nitrobenzaldehyde and 10.0mL of acetaldehyde into the three-necked flask, add 10mL of 30% potassium hydroxide-methanol solution in the dropping funnel, stir magnetically, and cool the reaction with an ice-salt bath bottle, when the temperature drops to 0ˉ5°C, slowly add 5mL potassium hydroxide-methanol solution dropwise under magnetic stirring, react for 40 minutes, then add 5mL potassium hydroxide-methanol solution dropwise, continue to react at about 10°C for 40 minutes, and cool down at 5°C The following reaction mixture is solidified, add 16 mL of acetic anhydride, heat on a water bath for 30 minutes, pour into 120 mL of hot water, add 16 mL of concentrated hydrochloric acid, heat in a water bath for 20 minutes, and let stand for 24 hours. Crystals were precipitated, filtered with suction, washed, and recrystallized in 30% aq...
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