A kind of preparation method of palbociclib intermediate
A technology of intermediates and compounds, applied in the field of drug synthesis, can solve problems such as unfavorable intermediates industrial production, difficult control of production costs, complex reaction products, etc., to avoid the use of heavy metal palladium catalysts, large implementation value, and reaction yield high effect
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[0030] 1) Preparation of compound II:
[0031] The ratio of compound I: 2,4-dichloropyrimidine, cyclopentylamine and triethylamine is =1:1:1.2
[0032] Add (1490g, 10.0mol) 2,4-dichloropyrimidine and 3L ethanol to a 10L four-neck flask, control the temperature in an ice-water bath to not exceed 25°C, add (851g, 9.99mol) cyclopentylamine and (1215g, 12.0mol) dropwise ) a mixed solution of triethylamine, after the dropwise addition was completed, stir at room temperature for 1 h. After the reaction was detected by HPLC, 3 L of water was added, stirred at room temperature for 1 hour to precipitate a white solid, filtered, washed with water, and dried to obtain compound II: 1680 g of 2-chloro-N-cyclopentylpyrimidin-4-amine, yield: 85.0%, MS: m / z 199 (M+H) +
[0033] The hydrogen spectrum characterization of compound II: 1 H NMR (400MHz, CDCI 3 , δppm): 1.46-1.56 (m, 4H), 1.58-1.83 (m, 4H), 2.64 (m, 1H), 6.14 (d, 1H), 7.59 (s, 1H), 7.73 (d, 1H).
[0034] 2) Preparation of Com...
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