Phenylacetic Acid → HCID 18355594, Verbindung

Temperatur

135 °C

A mixture of (2-hydroxy-5-methoxyphenyl)-(4-hydroxyphenyl)-methanone (0.59 g, 2.42 mmol), acetic anhydride (1.15 ml, 12.1 mmol), triethylamine (0.44 ml, 3.16 mmol), and phenyl acetic acid (0.33 g, 2.42 mmol) was stirred at 135° C. for 18 h. The resulting orange coloured solution was poured into water (20 ml) and stirred for 3 h, and the resulting mixture of aqueous solution plus sticky solid was diluted with ethyl acetate (20 ml) to dissolve the solid, and the organic layer separated. The aqueous phase was further extracted with ethyl acetate (2×20 ml). The combined organic extracts were washed with water, then brine, dried over sodium sulfate and evaporated to give a yellow/orange gum. This gum was dissolved in a minimum of ether and petrol added to precipitate the title compound as an off white powder.

1. stirringstirred for 3 h
2. additionthe resulting mixture of aqueous solution plus sticky solid
3. dissolutionto dissolve the solid
4. customthe organic layer separated
5. extractionThe aqueous phase was further extracted with ethyl acetate (2×20 ml)
6. washThe combined organic extracts were washed with water
7. dry with materialbrine, dried over sodium sulfate
8. customevaporated
9. customto give a yellow/orange gum
10. additionadded
11. customto precipitate the title compound as an off white powder

ORD-Eintrag

ord-c43eddd82f8748838b9354277ca95a7e

Quelldatensatz

uspto-grants-1999_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05958967