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Preparation method of Boc-glycine

A glycine, boc- technology, applied in chemical instruments and methods, cyanide reaction preparation, preparation of organic compounds and other directions, can solve the problems of insufficient environmental protection and safety in production, time-consuming and labor-intensive purification procedures, and increased production costs, and achieves low cost, Simple method and less pollution

Inactive Publication Date: 2015-01-14
CHONGZHOU HERUI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, glycine has a wide range of uses and effects, and in the prior art, using Boc as a protecting group to protect glycine is an important intermediate raw material for various medicines and biotechnology, and the existing methods for preparing Boc-glycine are all There are certain defects and certain limitations, so that the production is not environmentally safe, the yield is low, and impurities are easy to be produced. The subsequent purification process is time-consuming and laborious, which increases the production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Add 18.1g L-glycine and 100ml water into the reaction flask and stir. Add 0.01mol / L lye configured with 16g of sodium hydroxide to make it alkaline. Then add 8g of (Boc) 2 O reacted for 2 hours, then added 8g of (Boc) 2 O reacted for 2 hours, and finally added 9g of (Boc) 2 O was reacted for 4 hours.

[0027] 2. Use n-hexane 12ml / time to extract impurities three times. After adjusting the pH to 3 with 3mol / L hydrochloric acid, the product was extracted three times with dioxane 0.6L / time. The combined ester layers were washed with brine until neutral. Add 15 g of anhydrous sodium sulfate and dry for 10 hours.

[0028] 3. Filtrate, concentrate the filtrate to dryness under reduced pressure, add 60ml of n-hexane and stir to crystallize. The product is centrifuged and dried. 25.0 g of product was obtained. Yield 93.87%.

Embodiment 2

[0030] 1. Add 1kgL-glycine and 5.5L water into the reaction flask and stir. Add 0.05mol / L lye of 884g sodium carbonate configuration to adjust to alkaline. Then add 442g of (Boc) 2 O reacted for 5 hours, then added 442g of (Boc) 2 O reacted for 5 hours, and finally added 497g of (Boc) 2 O was reacted for 10 hours.

[0031] 2. Use n-hexane 600ml / time to extract impurities four times. After adjusting the pH to 3 with 6mol / L hydrochloric acid, the product was extracted four times with dioxane 1.2L / time. The combined ester layers were washed with brine until neutral. Add 300 g of anhydrous sodium sulfate and dry for 14 hours.

[0032] 3. Filtrate, concentrate the filtrate to dryness under reduced pressure, add 2.4L n-hexane and stir to crystallize. The product is filtered off and dried. The product 1512g was obtained. Yield 94.80%.

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PUM

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Abstract

The invention provides a preparation method of Boc-glycine. The preparation method comprises the steps of mixing a water solution of L-glycine and a water solution of sodium hydrogen carbonate; adding (Boc)2O in batches; and controlling reaction conditions to obtain Boc-glycine with high yield. The preparation method is low in cost, simple, convenient, safe in operation, little in pollution, high in yield and capable of easily realizing industrial production. The invention provides a novel method for industrial production of Boc-glycine.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing Boc-glycine. Background technique [0002] Boc-glycine is mainly used in the synthesis of peptides, mainly in a variety of pharmaceutical and biotechnology applications. [0003] Glycine, also known as aminoacetic acid, is a non-essential amino acid for the human body. Glycine is the simplest structure in the amino acid series, an amino acid that is not necessary for the human body. It has both acidic and basic functional groups in the molecule. It can be ionized in water and has strong hydrophilicity. It is a polar amino acid and is soluble in polar amino acids. Solvents, but insoluble in non-polar solvents, and has a higher boiling point and melting point. [0004] It can be used in the treatment of myasthenia gravis and progressive muscle atrophy; in the treatment of hyperesteridemia and chronic enteritis (combined with antacids); in combin...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/16
Inventor 郑果
Owner CHONGZHOU HERUI TECH
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