Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 62257-15-2, name is 2-Fluoro-5-methoxyaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Fluoro-5-methoxyaniline
Compound 36 (1eq.) Was dissolved in acetone was added KOH (4eq.), Was added with stirring dimethyl sulfate (1.5eq.), The reaction was stirred for 1 hour, then added 1ml of water and stirred for 1.5h. After completion of the reaction with ethyl acetate, dried over anhydrous magnesium sulfate, and purified by silica gel column chromatography to give intermediate 37.Intermediate 37 (1eq.) Was dissolved in glacial acetic acid, and then the acrylic acid (2eq.) Was added dropwise, with stirring was added 98% sulfuric acid (0.1eq.), 80 heated 5h. After completion of the reaction, saturated sodium bicarbonate solution and extracted with ethyl acetate, the organic phase was dried over anhydrous magnesium sulfate, and purified by silica gel column chromatography to give intermediate 38.Intermediate 38 (1mmol) was dissolved in 6mlEaton’s reagent, and the reaction was heated to 65 deg.] C overnight. After completion of the reaction with sodium hydroxide solution and extracted with ethyl acetate, the organic phase was dried over anhydrous magnesium sulfate, and purified by silica gel column chromatography to give intermediate 39.Compound 39 (1eq.) Was dissolved in anhydrous dichloromethane, the reaction flask was replaced with argon, -78 deg.] C was added BBr3 (5eq.), Gradually warmed to room temperature, the reaction for 5h, quenched with saturated sodium bicarbonate solution and neutralized, extracted with ethyl acetate, the organic phase was dried, purified by silica gel column chromatography to give intermediate 40.Compound 40 (1eq.) Was dissolved in acetone, was added Cs2CO3 (6eq.), Chloromethyl methyl ether was added to the strict (3eq.) The reaction flask under a nitrogen atmosphere with ice bath, the temperature was raised to 10 , the reaction 2h. After completion of the reaction and the reaction with 2N hydrochloric acid, extracted with ethyl acetate, and purified by silica gel column chromatography, the organic phase was dried, to give intermediate 41.Compound 41 was dissolved in anhydrous tetrahydrofuran, -40 deg.] C was added LDA (2eq.), Half an hour later butyryl chloride (1.1eq.), And the reaction warmed to room temperature, the reaction 0.5h, water was added to quench the reaction, under reduced pressure spin down tetrahydrofuran, extracted with ethyl acetate, the organic phase was dried after pressing down spin solvent, the crude product is dissolved in ethanol was added hydrazine hydrate (3eq.), 60 reaction 2h. After completion of the reaction was purified by silica gel chromatography to give intermediate 42 by column.Compound 42 (1eq.) Was added to trifluoroacetic acid, stirred at room temperature 1h, after completion of the reaction, the solvent under reduced pressure to spin dry, and the crude product was purified by silica gel column chromatography to give the desired product 43.Compound 43 was dissolved in dry tetrahydrofuran, was added sodium borohydride (5 eq.), Stirred at room temperature 3h, after completion of the reaction, water was added to quench the reaction, under reduced pressure of tetrahydrofuran spin down, extracted with ethyl acetate, dried over anhydrous magnesium sulfate purification by silica gel column chromatography to give compound KQ77.
The synthetic route of 62257-15-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Tsinghua University; He, Wei; Ruan, Ke; (60 pag.)CN105523955; (2016); A;,
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