Water → (4,5-Dichloro-2-methoxyphenyl)methanol

Temperatur

-20 °C

To a mixture of LiAlH4 (2.42 g, 64 mmol) in THF (40 mL) at −40° C. under argon, a solution of methyl 4,5-dichloro-2-methoxybenzoate (6 g, 26 mmol) in THF (50 mL) was added dropwise. The reaction mixture was stirred at −5° C. to 5° C. for 1 h. The mixture was cooled to −20° C. and then water (2 mL) and NaOH (15%) aqueous were added. The resulting mixture was stirred for 15 min. The solid was filtered, and the cake rinsed with ethyl acetate. The combined filtrate was dried over Na2SO4 and concentrated in vacuo to afford the crude product (4.6 g).

1. stirringThe resulting mixture was stirred for 15 min
2. filtrationThe solid was filtered
3. washthe cake rinsed with ethyl acetate
4. dry with materialThe combined filtrate was dried over Na2SO4
5. concentrationconcentrated in vacuo

ORD-Eintrag

ord-14093d7cd0e14a45b06610b6363a47ca

Quelldatensatz

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09227978B2