Preparation method of glycyl-tyrosine
A technology of glycyl chloride hydrochloride and tyrosine, applied in the direction of peptides, etc., can solve the problems of difficulty in drug production verification, inability to industrialize production, environmental hazards, etc., achieve low cost, reduce pollution, and avoid the use of organic solvents Effect
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Embodiment 1
[0021] A. Preparation of glycyl chloride hydrochloride: Put glycine (1.0Kg) and thionyl chloride (3.0Kg) into a 10L reaction kettle, heat to micro-reflux reaction for 6-8 hours, and distill off excess dichloride under reduced pressure Sulfoxide was added with isopropyl ether for beating, and centrifuged to obtain glycyl chloride hydrochloride (1.6Kg), with a yield of 90%.
[0022] B. Preparation of glycyl-tyrosine: Dissolve tyrosine (1.0Kg) in water (8.0Kg), slowly add potassium carbonate (3.8Kg), cool down to -5°C, add glycyl chloride in batches Salt (1.1Kg), the temperature is controlled within 10°C during the process, after the addition is completed, the reaction is incubated at 0-5°C for 3-5 hours, and no tyrosine is detected to indicate that the reaction is complete. The pH value was adjusted to 4.3-5.0 with dilute hydrochloric acid (3N), and 1.15 Kg of crude glycyl-tyrosine was obtained by filtration, with a yield of 88%.
[0023] C. Refining of glycyl-tyrosine: Suspend...
Embodiment 2
[0026] A. The preparation of glycyl chloride hydrochloride is the same as in Example 1.
[0027] B. Preparation of glycyl-tyrosine: Dissolve tyrosine (1.0Kg) in water (8.0Kg), add ethanol (2.0Kg), slowly add triethylamine (2.8Kg), cool to -10°C , add glycyl chloride hydrochloride (1.1Kg) in batches, control the temperature within 10°C during the process, after the addition is complete, keep the reaction at 0-15°C for 3-5 hours, and detect no tyrosine to show that the reaction is over. The pH value was adjusted to 4.3-5.0 with dilute hydrochloric acid (3N), and 1.18 Kg of crude glycyl-tyrosine was obtained by filtration, with a yield of 90%.
[0028] C. Refining of glycyl-tyrosine, same as embodiment 1. 0.93Kg of the refined product was obtained, the yield was 78.8%, and the content (HPLC) was 98.5%. Mp.278-285°C (dec), 1HNMR is the same as in Example 1.
Embodiment 3
[0030] A. The preparation of glycyl chloride hydrochloride is the same as in Example 1.
[0031] B. Preparation of glycyl-tyrosine: Dissolve tyrosine (1.0Kg) in water (8.0Kg), add DMF or tetrahydrofuran (2.0Kg), slowly add N-methylmorpholine (2.8Kg), Cool down to -10°C, add glycyl chloride hydrochloride (1.1Kg) in batches, control the temperature within 10°C during the process, complete the addition, keep it at 10-25°C for 3-5 hours, and detect no tyrosine to show the reaction End. The pH value was adjusted to 4.3-5.0 with dilute hydrochloric acid (3N), and 1.08 Kg of crude glycyl-tyrosine was obtained by filtration, with a yield of 82%.
[0032] C. Refining of glycyl-tyrosine, same as embodiment 1. 0.83Kg of the refined product was obtained, the yield was 76.8%, and the content (HPLC) was 98.2%. Mp.278-285°C (dec), 1HNMR is the same as in Example 1.
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