Water → Ethyl 2-[3-(Allyloxycarbonylmethyl)phenoxy]-2-methylpropionate

Temperatur

80 °C

Allyl 3-hydroxyphenylacetate (5.72 g, 32.9 mmol), potassium carbonate (6.82 g, 49.35 mmol), and ethyl 2-bromoisobutyrate (7.35 mL, 49.35 mmol) were dissolved in dimethylformamide (10 mL), and the mixture was stirred for 60 hours at 80° C. The reaction mixture was added to water, and the resultant mixture was extracted with diethyl ether, followed by washing sequentially with water and saturated brine, drying over magnesium sulfate, concentration under reduced pressure, and purification by silica gel column chromatography (n-hexane/ethyl acetate=20/1), whereby the target compound was obtained (6.40 g, 20.90 mmol, 63.5%).

1. extractionthe resultant mixture was extracted with diethyl ether
2. washby washing sequentially with water and saturated brine
3. dry with materialdrying over magnesium sulfate, concentration under reduced pressure, and purification by silica gel column chromatography (n-hexane/ethyl acetate=20/1), whereby the target compound
4. customwas obtained (6.40 g, 20.90 mmol, 63.5%)

ORD-Eintrag

ord-4cf418e2ef3b4c088a062f802b078c86

Quelldatensatz

uspto-grants-2003_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06653334B1