Iodoethane → 2-(2-Bromo-5-methoxy-phenyl)-2-ethyl-butyric acid

Temperatur

140 °C

(2-Bromo-5-methoxy-phenyl)-acetic acid methyl ester (3.51 g, 13.5 mmol) was dissolved in DMF (4.5 ml), and added with NaH (2.1 g, 67.7 mmol). Subsequently, 15-crown-5 (1.38 ml, 6.8 mmol) and EtI (5.5 ml, 67.7 mmol) cooled to 0° C. were added to the mixture. The mixture was diluted with ethyl acetate and washed with water and saturated brine. The residues obtained after concentration under reduced pressure were purified by silica gel column (hexane-ethyl acetate). Then, the resultant was dissolved in ethanol (80 ml) and water (80 ml), added with KOH (91 g), and stirred at 140° C. The reaction solution was extracted with ethyl acetate, and washed with water and saturated brine. After concentration under reduced pressure, the target compound was obtained (10.62 g, 78%).

1. additionwere added to the mixture
2. washwashed with water and saturated brine
3. customThe residues obtained
4. concentrationafter concentration under reduced pressure
5. customwere purified by silica gel column (hexane-ethyl acetate)
6. dissolutionThen, the resultant was dissolved in ethanol (80 ml)
7. additionwater (80 ml), added with KOH (91 g)
8. extractionThe reaction solution was extracted with ethyl acetate
9. washwashed with water and saturated brine
10. concentrationAfter concentration under reduced pressure
11. customthe target compound was obtained (10.62 g, 78%)

ORD-Eintrag

ord-515fd476b674485e96f072808d02c3a4

Quelldatensatz

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09126931B2