Preparation method of Pralatrexate suitable for industrial large scale production
A synthetic method and industrial technology, applied in the field of preparation and purification of the antineoplastic drug pralatrexate raw material and its important intermediates, can solve the problems of difficult reaction and post-processing, low yield and purity, etc., and achieve the goal of reaction Post-processing is simple and feasible, with high purity and the effect of reducing side reactions
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[0035] The present invention will be further described below by specific examples.
[0036] Step 1 Synthesis of intermediate 4-methyl formate methyl phenylacetate (B)
[0037] Add 80.0g of p-carboxyphenylacetic acid to a 2 L reactor, stir to dissolve with 800 mL of anhydrous methanol, add 8.0g of p-toluenesulfonic acid, stir and heat to reflux for 24 hours, spin off the methanol under reduced pressure, and add 240 mL of water to the residue , Extract with ethyl acetate (240mL×3), combine the organic phases, wash the organic phase with 3% NaOH solution (80mL×2), and then dry with anhydrous sodium sulfate. The solvent was recovered under reduced pressure and cooled to obtain compound B as a white solid. Weight: 84.1g, yield: 91.1%, HPLC content: 97.8%.
[0038] The proton nuclear magnetic spectrum data is as follows:
[0039] 1 H NMR (300 MHz, CDCl 3 )Δ 7.91(d, J = 6.3 Hz, 2H), 7.42(d, J = 6.3 Hz, 2H), 3.84(s, 3H), 3.79(s, 2H), 3.62(s, 3H).
[0040] Step 2 Synthesis of intermediate...
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