Aluminium lithium hydride → 4,4,4-Trifluoro-3-methylbut-2-en-1-ol

Temperatur

0 °C

Benzyl 4,4,4-trifluoro-3-methylbut-2-enoate (1.87 g, 7.67 mmol) in diethyl ether (5 mL) was added dropwise to a suspension of LAH (291 mg, 1.67 mmol) in diethyl ether (10 mL). After stirring at −78° C. for 10 min and at 0° C. for a further 30 min, the reaction mixture was filtered through cotton, quenched with sodium potassium tartrate and stirred vigorously until layers separated. The aqueous phase was extracted with diethyl ether. The combined ethereal layers were dried (magnesium sulfate) and concentrated in vacuo to afford 4,4,4-trifluoro-3-methylbut-2-en-1-ol which was used in the subsequent step without further purification.

1. filtrationthe reaction mixture was filtered through cotton
2. customquenched with sodium potassium tartrate
3. stirringstirred vigorously until layers
4. customseparated
5. extractionThe aqueous phase was extracted with diethyl ether
6. dry with materialThe combined ethereal layers were dried (magnesium sulfate)
7. concentrationconcentrated in vacuo

ORD-Eintrag

ord-295441accd164288aafa18b584f013ac

Quelldatensatz

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08318767B2