Method for synthesizing o-aminophenylpropyl alcohol
A technology of o-aminophenylpropanol and a synthetic method, applied in the field of synthesis of o-aminophenylpropanol, can solve the problems of high price of o-nitrocinnamyl alcohol, complicated operation of reaction equipment, etc., and achieves the requirements of low equipment requirements and simple operation. Effect
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example 1
[0020] (1) In a 25 ml two-necked round-bottomed flask equipped with a reflux condenser, add 0.137 grams (1 mmol) of o-nitrotoluene, 0.1851 grams (1.04 mmol) of N-bromosuccinimide, and 0.122 g (0.05 mmol) of benzoyl oxide and 10 ml of carbon tetrachloride were stirred and heated to reflux for 6 hours. After the reaction was finished, wash with hot carbon tetrachloride (2×10 ml), and the filtrate evaporated the solvent under reduced pressure with a rotary evaporator, and column chromatography (petroleum ether:ethyl acetate=10:1) gave a light yellow solid that was o-nitrobenzyl bromide.
[0021] (2) 25 ml two-necked bottle with 5 ml dropping funnel, add potassium tert-butoxide 0.1234 (1.1 mmol), 8 ml tetrahydrofuran, stir under ice-water bath, add propylene glycol dissolved in 2 ml tetrahydrofuran after the temperature drops Acetyl dimethyl ester 0.1585 g (1.2 mmol), stirred for half an hour. Slowly add 0.216 g (1 mmol) of o-nitrobenzyl bromide dissolved in 5 ml of tetrahydrofu...
example 2
[0026] (1) In a 50 ml two-necked round-bottomed flask equipped with a reflux condenser, add 1.37 grams (10 mmol) of o-nitrotoluene and 1.851 grams (10.4 mmol) of N-bromosuccinimide. 1.22 g (0.5 mmol) of benzoyl oxide and 25 ml of carbon tetrachloride were stirred and heated to reflux for 6 hours. After the reaction was finished, wash with hot carbon tetrachloride (2×20 ml), and the filtrate evaporated the solvent under reduced pressure with a rotary evaporator, and column chromatography (petroleum ether: ethyl acetate=10:1) gave a pale yellow solid that was o-nitrobenzyl bromide.
[0027] (2) 50 ml of two-necked bottle with 10 ml of dropping funnel, add potassium tert-butoxide 1.234 (11 mmol), 25 ml of tetrahydrofuran, stir under ice-water bath, add propylene glycol dissolved in 3 ml of tetrahydrofuran after the temperature drops Acetyl dimethyl ester 1.585 g (12 mmol), stirred for half an hour. Slowly add 2.16 g (10 mmol) of o-nitrobenzyl bromide dissolved in 8 ml of tetrah...
example 3
[0032] (1) In a 1-liter two-necked round-bottomed flask equipped with a reflux condenser, add 137 grams (1 mole) of o-nitrotoluene, 185.1 grams (1.04 moles) of N-bromosuccinimide, and benzene peroxide 122 g (0.05 mol) of formyl and 600 ml of carbon tetrachloride were stirred and heated to reflux for 7 hours. After the reaction was finished, wash with hot carbon tetrachloride (2×200 ml), and the filtrate evaporated the solvent under reduced pressure with a rotary evaporator, and recrystallized with a solvent (petroleum ether:ethyl acetate=10:1) to obtain a light yellow solid That is, o-nitrobenzyl bromide.
[0033] (2) 1 liter of two-necked bottle with 200 ml of dropping funnel, add potassium tert-butoxide 123.4 (1.1 mol), 500 ml of tetrahydrofuran, stir under ice-water bath, add malonic acid dissolved in 50 ml of tetrahydrofuran after the temperature drops 158.5 g (1.2 mol) of dimethyl ester was stirred for 1 hour. Slowly add 216 grams (1 mole) of o-nitrobenzyl bromide disso...
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