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2-(3-methoxyphenyl)-2-methylpropan-1-ol synthesis

4synthesis methods
-

Yield:17653-95-1 93 %

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran at 20;Inert atmosphere;Cooling with ice;

Steps:

66.xxvii

Add 2.1g43-A (10.9mM, 1.0eq) into a 250mL eggplant-shaped bottle,Add 100mLTHF to dissolve it completely, and after argon replacement, slowly add 21.8mLLiAlH4 THF solution (1.0MinTHF, 21.8mM, 2.0eq) dropwise under ice bath,React at room temperature for 1 h, add sodium sulfate decahydrate to the flask to quench the reaction solution,Until no obvious bubbles are formed, slowly add 1N sodium hydroxide aqueous solution dropwise to it,Until a large amount of precipitate is formed, filter, and the filter cake is washed with ethyl acetate,The obtained filtrate was extracted with ethyl acetate (50mL×3) and water (30mL), and the combined organic phases were obtained.After drying with anhydrous sodium sulfate and filtering, the filtrate was concentrated to obtain a yellow oil.After separation by silica gel column chromatography (PE/EA=10/1), 1.82 g of colorless oily liquid 44-A was obtained.Yield: 93.0%.

References:

CN115677719,2023,A Location in patent:Paragraph 0532-0535; 0540