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Method for preparing L-serine-15N

A technology of -15N, serine, applied in the field of preparation of L-serine-15N, to achieve the effect of high utilization

Inactive Publication Date: 2011-05-11
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Above synthetic method, there is no comparatively suitable preparation L-serine- 15 N approach, need to explore new L-serine- 15 The synthesis route of N, and improve the synthesis process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 0.3mol Na 15 N0 2(the abundance is 99.3%), 0.3mol diethyl malonate, 80ml toluene and 10g water were added in a 500ml three-necked flask and stirred evenly, the temperature of the reaction system was lowered to 5°C, and 1mol Acetic acid; the temperature was raised to 30°C and stirring was continued for 10 hours. Add toluene and water after completion of the reaction, obtain diethyl malonate-containing oximino through extraction and separation 15 The toluene phase of N is washed and dried and the toluene is removed by distillation under reduced pressure to obtain diethyl oximinomalonate- 15 N.

[0025] Diethyl oximinomalonate- 15 N, 0.4mol acetic acid, 0.8mol acetic anhydride and 2g of 5% Pd / C catalyst were added to a 500ml pressure-resistant reactor and stirred evenly, replaced with nitrogen and hydrogen 10 times respectively, and the reaction temperature was controlled at 40°C and the pressure at 0.1 MPa, continue to feed hydrogen to react for 10 hours. The solids...

Embodiment 2

[0029] 1mol Na 15 NO 2 (abundance is 99.3%), 0.3mol diethyl malonate, 40ml toluene and 4g water are added in the 500ml three-necked flask and stirred evenly, the temperature of the reaction system is lowered to 5 ℃, and 5mol Acetic acid; the temperature was raised to 30°C and stirring was continued for 10 hours. Add toluene and water after completion of the reaction, obtain diethyl malonate-containing oximino through extraction and separation 15 The toluene phase of N is washed and dried and the toluene is removed by distillation under reduced pressure to obtain diethyl oximinomalonate- 15 N.

[0030] Diethyl oximinomalonate- 15 N, 2mol acetic acid, 1.2mol acetic anhydride, and 8g of 5% Pd / C catalyst were added to a 500ml pressure-resistant reactor and stirred evenly, replaced with nitrogen and hydrogen 10 times respectively, and the reaction temperature was controlled to be 70°C and the pressure was 1.0MPa. Continue to feed hydrogen to react for 8 hours. The solids were...

Embodiment 3

[0034] 2mol Na 15 NO 2 (the abundance is 99.3%), 0.3mol diethyl malonate, 100ml toluene and 20g water are added in the 500ml three-necked flask and stirred evenly, the temperature of the reaction system is lowered to 5°C, and 2mol Acetic acid; the temperature was raised to 30°C and stirring was continued for 10 hours. Add toluene and water after completion of the reaction, obtain diethyl malonate-containing oximino through extraction and separation 15 The toluene phase of N is washed and dried and the toluene is removed by distillation under reduced pressure to obtain diethyl oximinomalonate- 15 N.

[0035] Diethyl oximinomalonate- 15 N, 1mol acetic acid and 0.4mol acetic anhydride were added to a 500ml pressure-resistant reactor and stirred evenly, and excessive zinc powder was added in batches for reduction reaction, the reaction temperature was controlled at 80°C, the pressure was normal pressure, and the reaction was carried out for 18 hours. The solid was removed by ...

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Abstract

The invention provides a method for preparing L-serine-<15>N, which comprises the following steps: adopting Na<15>NO2 and diethyl malonate as raw materials to synthesize acetamino-diethyl malonate-<15>N; using the obtained acetamino-diethyl malonate-<15>N to synthesize N-acetyl-DL-serine-<15>N; detaching through enzyme method to obtain the L-serine-<15>N. The utilization rate of the <15>N raw material of the inventive preparation method is high, the optical purity of the purified product L-serine-<15>N is more than 98. 5% and the chemical purity is more than 98%, and the <15>N abundance in the product is more than 98%.

Description

technical field [0001] The present invention relates to the preparation method of the organic compound labeled with stable isotope, relate in particular to a kind of L-serine- 15 N preparation method. Background technique [0002] Nitrogen-15 (referred to as 15 N, the same below) is a stable isotope of nitrogen, 15 N markers can be used as tracers and are widely used in biochemistry, medicine, pharmacy, agricultural science and other fields, especially for life science research. Serine- 15 N can be used as a tracer to study metabolism in living organisms. Food added L-serine- 15 N injection can be used to study the metabolic pathway of serine in animals (Shemin, D., J.Biol.Chem., 1945,158:297; Elwyn, D., Sprinson, D.B., J.Biol.Chem., 1949,178 : 475), to study the relationship between L-serine metabolism and protein synthesis rate in the human body (Monica, C., David, H., Rapid Commun.Mass.Spectrum., 1995, 9 (8): 655-659; Stein, T.P. , Settle, R.G., Albina, J.A., Denps...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/22C07C227/00C07B59/00
Inventor 杨飞卢伟京杜晓宁徐建飞
Owner SHANGHAI RES INST OF CHEM IND
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