Process for preparing (+/-)-3-(Carbamoymethyl)-5-methylhexanoic acid
A technology of methylhexanoic acid and carbamoyl group is applied in the field of preparation of -3--5-methylhexanoic acid and achieves the effects of low cost, simple operation and high total yield
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Embodiment 1
[0014] Example 1 Preparation of 3-isobutylglutaric acid
[0015] Add 18.5g (0.22mol) of cyanoacetamide, 50g of water, and 0.5g of catalyst (DMF) into a four-neck flask equipped with a reflux condenser, a thermometer, a stirrer and a constant pressure dropping funnel, and cool to 5~15°C , Stir and add 8.6g (0.1mol) of isovaleraldehyde, react at 5~15°C for 8 hours, keep warm, cool, add 70g (0.7mol) of 98% sulfuric acid dropwise, control the internal temperature at 30~50°C, dropwise time 2~3 hours, add dropwise, keep warm at 30~50°C for 3 hours, then slowly raise the temperature to 70~80°C, keep warm for 1 hour, then raise the temperature to reflux, the temperature is 100~110°C, reflux reaction for 3 hours , then distill the water at normal pressure to an internal temperature of 130~135°C, stop distilling water, and reflux at this temperature for 3 hours. After the reaction, cool to 50~60°C, add 50ml of toluene, and stir at 50~60°C After 0.5~1 hour, it is static and stratifi...
Embodiment 2
[0016] Example 2 Preparation of 3-isobutylvaleric anhydride
[0017] In a four-necked flask equipped with a reflux condenser, a thermometer, and a stirrer, add 37.6 g (0.2 mol) of 3-isobutylglutaric acid glutaric acid and 30.6 g (0.3 mol) of acetic anhydride, raise the temperature to reflux, and keep reflux React for 3 hours. Then distill a part of acetic acid and acetic anhydride, stop the distillation after the internal temperature reaches 100~120°C, and keep the reaction at 120°C for 4 hours. After the reaction is completed, cool down to lower the temperature to below 80°C, turn on the vacuum, start vacuum distillation to remove the low boiling point, and start vacuum distillation to obtain 32 g of 3-isobutylvaleric anhydride, the HPLC content is 98.5%, and the yield is ≥90%.
Embodiment 3
[0018] The preparation of embodiment 3 (±)-3-(carbamoyl)-5-methylhexanoic acid
[0019] In a four-necked flask equipped with a thermometer and a stirrer, add 25 ml of methyl tert-butyl ether and 50 ml of water, and stir under 5° C., dropwise add 17 g of 3-isobutylvaleric anhydride prepared according to the method of Example 2 ( 0.1mol) and 22g (0.25mol) of ammonia water, the temperature is less than 0°C, after dripping, the pH=9, then control -5~0°C, keep warm for 4 hours, the pH remains unchanged, stand still for 0.5 hours, separate into layers, water layer Add 50ml of water, add 30wt% hydrochloric acid dropwise, control the temperature to less than 10°C, pH=1~2, discharge, filter to obtain 28g of crude wet product. The rough wet product is refined, and the method is as follows: After heating and dissolving 28g of the thick wet product with 280g methyl tert-butyl ether, divide the water, add 3g of activated carbon for decolorization, filter, cool and crystallize, filter, ...
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