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With sulfuric acid; In dichloromethane; at 20℃; for 120h;
3. Add 390 g of about 12 g of CH2Cl2 (dichloromethane), concentrated H2SO410.5 g and Z-L-Tyr-OMe (N-benzyloxycarbonyl-L-tyrosine methyl ester) to the reaction flask.250 g of isobutene was added, and the reaction was stirred at room temperature for 5 days. The reaction was equilibrated and the TLC (thin layer chromatography) detection reaction was completed.After completion of the reaction, 100 g of NaOH solution having a concentration of 30% was added and saponified. After saponification was complete, the layers were allowed to stand, and the organic layer was concentrated in hot water to CH2Cl2 (dichloromethane), 300 g of AcOEt (ethyl acetate) The ester layer was washed several times with saturated brine and 10 g of liquid caustic solution.Adjust the pH to 3 with citric acid. And then washed several times with saline, add activated carbon 5g decolorization, filter in addition to activated carbon.Vacuum hot water to concentrate the ester layer to dry, add methanol 500g, water 40g, add activated carbon 3g decolorization filter,Z-L-Tyr (tBu) (N-benzyloxycarbonyl-O-tert-butyl-L-tyrosine) was obtained and added to a hydrogenolysis vessel.
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