Compound for preparation of 4 - (10 B) dihydroxy boryl- L - phenylalanine
A technology of phenylalanine and hydroxyboron, which is applied in the field of compounds used to prepare 4-(10B) dihydroxyboron-L-phenylalanine, and can solve problems such as difficulty in preparation, inability to apply to preparation, etc.
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[0018] (1) Prepare (S)-N-tert-butoxycarbonyl- 4-( 10 B) Dihydroxyboryl phenylalanine
[0019]
[0020]
[0021] First, a 3-liter three-necked bottle equipped with a mechanical stirrer, a thermometer, and a nitrogen inlet joint sealed with a rubber gasket was prepared. Inject 750 milliliters of 2-methyltetrahydrofuran into the three-necked flask, then add 128 millimoles (50.0 grams, 100% purity) of (S)-N-tert-butoxycarbonyl-4-iodophenylalanine, And the two were uniformly stirred to form a solution; after that, 393 mmol (90.1 g, 106 ml) of 10 Tributyl borate was added to the solution to form a mixed solution.
[0022] Next, the mixed solution was cooled to between -85°C and -76°C, and a 1.6M (600 mmol, 375 ml) hexane solution of n-butyllithium (n-butyllithium) was added dropwise to the mixture over 3 hours. Mix the solutions to obtain a reaction mixture.
[0023] Then, the reaction mixture was stirred at -80°C for 0.5 hours, and a small amount of the reaction mixture ...
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