Hydrochloric Acid → HCID 10337891, Verbindung

Temperatur

0 °C

To a suspension of lithium aluminum hydride (350 mg) in diethyl ether (10 ml) was added dropwise, at 0° C., a solution of ethyl 4-[4-[2-[(E)-2-phenylethenyl]-4-oxazolylmethoxy]phenyl]butyrate (3.00 g) in diethyl ether (10 ml)—tetrahydrofuran (10 ml). The mixture was stirred at 0° C. for one hour and at room temperature for further one hour, followed by addition of water. The mixture was acidified with 2N hydrochloric acid and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography. From the fraction eluted with ethyl acetate-hexane (1:1,v/v), 4-[4-[2-[(E)-2-phenylethenyl]-4-oxazolylmethoxy]phenyl]butanol (2.00 g, 74%) was obtained. Recrystallization from ethyl acetate-hexane afforded colorless needles, mp 90-91° C.

1. additionwas added dropwise, at 0° C.
2. extractionextracted with ethyl acetate
3. washThe ethyl acetate layer was washed with water
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. washFrom the fraction eluted with ethyl acetate-hexane (1:1,v/v)

ORD-Eintrag

ord-fb01c660f4aa4634aea045a458ac458f

Quelldatensatz

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06211215B1