Method for using glyceric acid to prepare 3-hydroxypropionic acid
A technology of hydroxypropionic acid and glyceric acid, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of complicated operation and high cost, and achieve simple reaction system, low cost and product selectivity. high effect
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Embodiment 1
[0021] In a 50 mL high temperature and high pressure reactor, 4 mmol glyceric acid and 100 μmol PdCl were sequentially added 2 , 10 ml of 30wt% hydriodic acid, sealed the reactor, filled with hydrogen (400 psi), stirred and rapidly heated to 100°C, and kept for 10 h. The reactor was cooled to room temperature in an ice-water bath, and the aqueous phase was collected and detected. The conversion rate of glyceric acid was 100%, and the yield of 3-iodopropionic acid was 99%. Take 5 ml of the aqueous phase reactant, add 10 ml of n-hexanol to extract 2-iodopropionic acid, extract three times, and combine the extractants. Take 10 ml of extract and 10 ml of water into a 50 mL pressure-resistant reactor, and add 0.15 g of sodium hydroxide, seal the reactor, stir and rapidly heat to 80 °C for 2 h. The reactor was cooled to room temperature in an ice-water bath, and the aqueous phase was collected, acidified and detected. The yield of 3-hydroxypropionic acid was 99%.
[0022] The dete...
Embodiment 2
[0031] Add 4 mmol glyceric acid, 0.2 g Pd / C (loading capacity 5wt%), and 10 ml 30wt% hydroiodic acid successively into a 50 mL high-temperature and high-pressure reactor, seal the reactor, fill it with hydrogen (400 psi), stir and quickly Heated to 100°C and kept for 10h. The reactor was cooled to room temperature in an ice-water bath, and the aqueous phase was collected and detected. The conversion rate of glyceric acid was 100%, and the yield of 3-iodopropionic acid was 99%. Take 10 ml of the aqueous phase reactant, add 10 ml of n-hexanol to extract 2-iodopropionic acid, extract three times, and combine the extractants. Take 10 ml of extract and 10 ml of water into a 50 mL pressure-resistant reactor, add 0.15 g of sodium hydroxide, seal the reactor, stir and rapidly heat to 80 °C for 2 h. The reactor was cooled to room temperature in an ice-water bath, and the aqueous phase was collected, acidified and detected. The yield of 3-hydroxypropionic acid was 99%.
Embodiment 3
[0033] Add 4 mmol glyceric acid, 0.2 g Rh / C (loading capacity 5wt%), and 10 ml 20wt% hydroiodic acid to a 50 mL high-temperature and high-pressure reactor in sequence, seal the reactor, fill it with hydrogen (400 psi), stir and quickly Heat to 80°C and keep for 20 h. The reactor was cooled to room temperature in an ice-water bath, and the aqueous phase was collected and detected. The conversion rate of glyceric acid was 100%, and the yield of 3-iodopropionic acid was 99%. Take 5ml of the aqueous phase reactant, add 10ml of n-hexanol to extract 2-iodopropionic acid, extract three times, and combine the extractants. Take 10 ml of extract and 10 ml of water into a 50 mL pressure-resistant reactor, add 0.15 g of sodium hydroxide, seal the reactor, stir and rapidly heat to 80 °C for 2 h. The reactor was cooled to room temperature in an ice-water bath, and the aqueous phase was collected, acidified and detected. The yield of 3-hydroxypropionic acid was 99%.
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