Kyotorphin modified fatty amine/alcohol derivative, and preparation method and application thereof
A compound and anti-inflammatory drug technology, applied in the field of artificially synthesized polypeptide compounds, can solve the problems of poor oral activity
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Embodiment 1
[0021] Example 1 prepares N G -Arg(NO 2 )
[0022] Under the condition of ice-salt bath stirring, add 80ml concentrated nitric acid to 500ml eggplant bottle, then slowly add 80ml concentrated sulfuric acid. After 10 min, 47.33 g (272 mmol) of L-Arg was added in batches, and the reaction mixture was stirred and reacted for 2 h in an ice-salt bath. Slowly add 96ml of ice water to the reaction mixture, then slowly add concentrated ammonia water, adjust the pH to 8, then adjust the pH to 6 with glacial acetic acid, a large amount of colorless solid precipitates, put it in a refrigerator at 4°C to continue crystallization. Filter under reduced pressure, discard the filtrate, dissolve the filter cake with hot water at 80°C, and put it in a refrigerator at 4°C for recrystallization. Filter under reduced pressure at room temperature to collect 52.5 g of insoluble matter as a colorless solid with a yield of 88%. ESI-MS (m / e): 220 [M+H] + .
Embodiment 2
[0023] Embodiment 2 prepares N α -Boc-N G -Arg(NO 2 )
[0024] Weigh 1.752g (8mmol) N G -Arg(NO 2 ) into the reaction bottle, add 3ml of water to dissolve, under the condition of ice bath, slowly add 8ml of 1N NaOH dropwise, will dissolve 1.92g (Boc) 2 Slowly pour the dioxane of O into it, adjust the pH of the reaction solution to 9, and react for 48 hours. During this period, the CO in the reaction system is pumped every 2 hours 2 once. After the reaction is complete as detected by TLC, adjust the pH of the reaction solution to 7, spin off dioxane, then adjust the pH of the reaction solution to 2, extract the reaction solution three times with ethyl acetate, and then wash the ethyl acetate layer three times with saturated NaCl , to obtain the ethyl acetate layer with anhydrous NaSO 4 Dry overnight, filter to remove NaSO 4 , spin-dried ethyl acetate to obtain 2.4 g of the title compound as a colorless solid, yield 94%. ESI-MS (m / e): 320 [M+H] + .
Embodiment 3
[0025] Embodiment 3 prepares N G -Arg(NO 2 )-OBzl
[0026] Take 6.57g (30mmol) N G -Arg(NO 2 ) into the reaction flask, then add 6.21g of sodium benzenesulfonate, 50ml of benzyl alcohol, and 20ml of cyclohexane, and react in an oil bath at 80°C for 8h. , to obtain 14.1 g of the title compound as a colorless solid, with a yield of 98%. ESI-MS (m / e): 310 [M+H] + .
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