Method for synthesizing bursa of Fabricius bursin
The technology of a bursalin and a synthetic method, which is applied in the field of synthesis of biological preparations, can solve the problems of low production cost, small amount of production, and difficulty in producing bursalin, and achieve reduction in production cost, increase in yield, and significant The effect of applying value
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Embodiment 1
[0029] (1), amino acid protection
[0030] a. Dissolve 13.1 g of lysine and 13.9 g of histidine in 50 ml of 2mol·1 -1 In NaOH, ice-salt bath, under stirring, add 34.1 g of Z-Cl pre-dissolved in THF dropwise, and at the same time add 2mol·1 -1 NaOH keeps the solution at pH=9. After the addition is completed, the temperature is naturally raised to room temperature, and the stirring is continued for 1 hour, washed twice with 50 ml of diethyl ether, and the ether layer is separated, and the water phase is added dropwise with 6 mol·1 -1 Hydrochloric acid to pH = 1, add 75 ml of ethyl acetate, continue to stir for 5 minutes, separate the layers, wash the ethyl acetate layer with 5% NaCl until neutral, anhydrous NaCl 2 SO 4 After drying, the solvent was distilled off under reduced pressure to obtain Z 2 -Lys and Z 2 -His;
[0031] b. Dissolve 5.9 g of glycine in 50 ml of methanol, put it in an ice-salt bath and cool to -10°C, slowly add 20 ml of thionyl chloride dropwise, then add...
Embodiment 2
[0046] (1), amino acid protection
[0047] a. Dissolve 13.1 grams of lysine and 13.9 grams of histidine in 50 milliliters of 2mol·l -1 In NaOH, ice-salt bath, add 22 g (Boc) dissolved in THF dropwise under stirring 2 O, while adding 2mol·l dropwise -1 NaOH kept the solution at pH=9. After the addition, it was naturally raised to room temperature, continued to stir for 1 hour, washed twice with 50 ml of ether, and the ether layer was separated, and the aqueous phase was added dropwise with 6 mol l -1 Hydrochloric acid to pH = 1, add 75 ml of ethyl acetate, continue to stir for 8 minutes, separate the layers, wash the ethyl acetate layer with 5% NaCl until neutral, anhydrous NaCl 2 SO 4 After drying, the solvent was distilled off under reduced pressure to obtain Z 2 -Lys and Z 2 -His;
[0048] b. Dissolve 5.9 g of glycine in 50 ml of methanol, put it in an ice-salt bath and cool to -10°C, slowly add 20 ml of thionyl chloride dropwise, then add 10 ml of 98% concentrated su...
Embodiment 3
[0063] (1), amino acid protection
[0064] a. Dissolve 13.1 grams of lysine and 13.9 grams of histidine in 50 milliliters of 2mol·l -1 In NaOH, ice-salt bath, add 22 g (Boc) dissolved in THF dropwise under stirring 2 O, while adding 2mol·l dropwise -1 NaOH keeps the solution at pH = 9. After the addition is complete, let it rise to room temperature naturally, continue to stir for 1 hour, wash twice with 50 ml of ether, separate the ether layer, and add 6 mol l of the aqueous phase dropwise under stirring. -1 Hydrochloric acid to pH = 1, add 75 ml of ethyl acetate, continue to stir for 6 minutes, separate the layers, wash the ethyl acetate layer with 5% NaCl until neutral, anhydrous NaCl 2 SO 4 Drying, removal of solvent by distillation under reduced pressure, to obtain Boc 2 -Lys and Boc 2 -His;
[0065] b. Dissolve 5.9 g of glycine in 50 ml of methanol, put it in an ice-salt bath and cool to -10°C, slowly add 20 ml of thionyl chloride dropwise, then add 10 ml of 98% con...
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