A prep work technique of L-Alanyl-L-Glutamine. The steps of the preparation technique are as adhere to:
1) Prep work of chloro-Boc-alanine: Include 18.9 g of Boc-alanine into the reaction container, then add 17.9 g of sulfoxide chloride, and afterwards consist of 0.7 g of N,N-dimethylformamide, mix at 75-85 ° C for 5 hours, after that awesome to 40-50 ° C, regulate the temperature level at 45-55 ° C and concentrate under reduced tension till there is no extract, and the oil obtained is used directly for the following action of the response;
2) Prep Work of Boc-alanylsuccinimide: Dissolve 13.8 g of N-hydroxysuccinimide in 90ml of acetone, after that include 50.5 g of triethylamine, and liquify chloro-Boc-alanylsuccinimide in an ice-water bathroom. Dissolve 0.1 mol of amino acid in 40 ml of acetone and include it dropwise to the above system. After the addition is overall, respond at location temperature level for 4 hours. After that add 400g of detoxified water to the reaction system. A huge quantity of strong will certainly speed up. Filter with suction. Wash the filter cake with detoxified water for 50 ℃ blast drying to get Boc-alanyl succinimide;
3) Prep Job of Boc-Proglutide: Add 10.2 g glutamine and 7mL water to the response container, after that include 10g ammonia water, mix till clear, then consist of 10ml ethanol, and dropwise add Boc-Protein liquified in 40ml ethanol under stirring conditions. For the system of aminoacyl succinimide, continue the reaction at area temperature degree for 2 hours after the dropwise addition; after that gradually include 2M hydrochloric acid dropwise right into the system, readjust the pH to 2 ~ 3, stir for 1 hour, and precipitate a wide variety of crystals, after that filter and completely dry to get white shade strong;
4) Prep Work of L-Alanyl-L-Glutamine: eliminate tert-butoxycarbonyl group. The treatment of removing the tert-butoxycarbonyl team is as complies with: consist of 60ml of methylene chloride and 20ml of trifluoroacetic acid to the reaction container containing 19.0 g of Boc-propylene glycol dipeptide, react at area temperature level for 5 hours, and afterwards consist of 50ml of methyl tert-butyl ether. The solid is precipitated, filteringed system with suction, and dried out to get solid proglutamine dipeptide.