A method for preparing 3-(2-thienyl)-d-alanine
A technology of alanine and thienyl group, applied in the field of preparing 3--D-alanine, can solve the problems of high cost, low yield, cumbersomeness and the like, and achieves the advantages of low production cost, high yield and reduced cost. Effect
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Embodiment 1
[0047]Embodiment 1, the preparation of the fermented liquid that contains D-hydantoin hydrolase and carbamoyl hydrolase
[0048] The specific fermentation conditions are: the enzyme-producing bacterium is Pseudomonas putida.2262 (purchased from Shanxi Institute of Microbiology), 1.0% glucose, 0.8% inducer, 2.5% corn steep liquor, 0.05% magnesium sulfate, 0.05% Sodium dihydrogen phosphate, 0.1% ammonium sulfate, 0.02% cobalt chloride. Use sodium hydroxide solution to adjust the pH to 7.0-7.2, the inoculation amount of the seed solution is 10% (v / v), culture at 30-32°C for 20-24 hours under the condition of 160 rpm, the microscopic examination is full, and the OD value is 0.6 ~0.8, enzyme activity: 0.5-0.6umol / (ml.min), collect the bacteria after high-speed centrifugation. The enzyme is an intracellular enzyme, does not need to break the wall, and the fermentation broth is used after centrifugation or centrifugation.
Embodiment 2
[0050] (1) Add 500ml of water into a 1000ml four-neck flask equipped with a stirring, ventilating and reflux device, then add 100g (1mol) hydantoin and 5g (0.08mol) ethanolamine, stir fully, protect with nitrogen, and keep warm in a water bath for 10 to 15 ℃, 106g (0.95mol) 2-thiophene formaldehyde was added dropwise, and the dropwise addition was completed in 2 hours. After the drop, the temperature was raised to 85°C, and the temperature was kept for 3 hours. It was detected that there was no 2-thiophene formaldehyde in the solution, and the temperature was continued to rise to 95°C. hour, cooled to room temperature, suction filtered, washed with a small amount of water, and dried to obtain 175.2 g of 2-thiophene hydantoin (95.5% yield, 99.3% purity);
[0051] (2) Add 400ml water in 1000ml autoclave, then add 40g (0.21mol) 2-thiophene hydantoin, 20g (0.5mol) sodium hydroxide and 5g palladium carbon catalyst (10wt%Pd / C), airtight, nitrogen Replace 3 times, then replace 3 time...
Embodiment 3
[0056] (1) Add 250ml of water in a 500ml four-neck flask with stirring, ventilating and reflux devices, then add 50g (0.5mol) hydantoin and 2.8g (0.036mol) n-propanolamine, fully stir, and protect with nitrogen, Keep warm in a water bath at 10-15°C, add 53g (0.475mol) 2-thiophene carboxaldehyde dropwise, and complete the dropwise addition in 2 hours. After the drop is completed, raise the temperature to 85°C and keep it warm for 3 hours. It is detected that there is no 2-thiophene carboxaldehyde in the solution, and continue to heat up to 95°C, keep warm for 1 hour, cool down to room temperature, filter with suction, wash with a small amount of water, and dry to obtain 87.4g of 2-thiophene hydantoin (95.3% yield, 99.1% purity);
[0057] (2) Add 400ml water in 1000ml autoclave, then add 40g (0.21mol) 2-thiophene hydantoin, 20g (0.5mol) sodium hydroxide and 5g palladium carbon catalyst (10wt%Pd / C), airtight, nitrogen Replace 3 times, then replace 3 times with hydrogen, control t...
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