Method for preparing L-(+)-alpha-phenylglycine
A technology of L-phenylglycine and phenylglycine, which is applied in the field of preparation of L-phenylglycine, can solve the problems of low equipment utilization, high production cost, and low product yield, and achieve high equipment utilization, low production cost, and high product yield. high effect
Inactive Publication Date: 2014-06-25
JINYIMENG GRP CO LTD
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Problems solved by technology
[0004] 1. The production cycle is long, the production cycle of a single batch can reach 24 hours, and the racemization time accounts for more than 75% of the entire production cycle
[0005] 2. The product yield is low, below 85%
[0006] 3. Low utilization rate of equipment and high production cost
Method used
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Embodiment 1
[0045] According to the preparation method of the present invention, L-phenylosylic acid is prepared, and the steps are as follows:
[0046] ①.Splitting and salting
[0047] Put 1 part by weight of DL-phenylglycine and 0.35-0.55 parts by weight of D-(+) camphorsulfonic acid into the resolution kettle 1, and carry out resolution and salt-forming reaction in dilute sulfuric acid aqueous solution, the reaction temperature is 90-105 °C, the reaction time is 0.5 to 1.5 hours;
[0048] ②.Centrifugal separation
[0049] The splitting and salt-forming reaction product of step ① is centrifuged through the double salt centrifuge 4, and the filter cake is transferred to the hydrolysis kettle 2 for alkali analysis and hydrolysis;
[0050] ③. Racemization, desalination
[0051] The centrifuged mother liquor from step ② is sent back to the split kettle 1 through the double salt mother liquor tank 6 and the double salt mother liquor pump 8, and an aqueous sodium hydroxide solution is adde...
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The invention discloses a method for preparing L-(+)-alpha-phenylglycine, which belongs to a carbocyclic compound of which the carbon skeleton has a hexatomic aromatic ring and an amino and a carboxyl which are bonded with the same non-ring carbon atom of the carbon skeleton. The invention particularly relates to a method for preparing L-(+)-alpha-phenylglycine by splitting D(-)-alpha-aminophenylacetic acid. The method is characterized by comprising the following process steps: 1, splitting and salifying; 2, performing centrifugal separation; 3, racemizing and desalting; 4, separating in alkali and dehydrating; 5, crystallizing and performing centrifugal separation; and 6, recycling filtrate. The method for preparing L-(+)-alpha-phenylglycine has the advantages of short production period, high product yield, high equipment utilization rate and low production cost. The single-batch production period of the method is 7 to 10 hours; and the final levorotatory form yield of the method is up to 95 percent which is 10 to 15 percent higher than that of the prior art. The equipment utilization rate is high, the production capacity is improved to two times that of the prior art, and thus, the production cost is reduced greatly.
Description
technical field [0001] The invention is a preparation method of L-phenylglycine. It belongs to the carbocyclic compound with a carbon frame containing a six-membered aromatic ring and an amino group and a carboxyl group connected to the non-ring carbon atom of the same carbon frame. It particularly relates to a method for preparing L-phenylglycine by splitting D-phenylglycine. Background technique [0002] The left-handed form of phenylglycine, D-(-)phenylglycine, or L-phenylglycine, is an important pharmaceutical intermediate and an important raw material for the synthesis of ampicillin, cephalexin, and L-dihydrophenylglycine. [0003] The preparation method in the prior art mainly uses the resolving agent D-(+) camphorsulfonic acid to resolve DL-phenylglycine. There are following deficiencies: [0004] 1. The production cycle is long, and the production cycle of a single batch can reach 24 hours, and the racemization time accounts for more than 75% of the entire product...
Claims
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IPC IPC(8): C07C229/36C07C227/34
Inventor 张超张立省王仕高马晓丽王怀利张金玲
Owner JINYIMENG GRP CO LTD