3-Methoxyphenol → Dimethyl-(3-methoxyphenoxy)malonate

To a solution of 3-methoxyphenol (115 g) in acetone (1000 ml) was added K2CO3 (115 g). The suspension was stirred at 40° C. for 15 min. A solution of dimethylchloromalonate (133 ml) in acetone was added over a period of 45 min. The resulting brown suspension was stirred overnight at 70° C. Finally, the solvent was removed under reduced pressure and the residue was taken up in water (1000 ml) and extracted twice with DCM (500 ml). The combined organic layers were washed with water (500 ml), dried over Na2SO4, and evaporated to give crude dimethyl-(3-methoxyphenoxy)malonate (230 g) as an orange oil. The product was not purified any further.

1. stirringThe resulting brown suspension was stirred overnight at 70° C
2. customFinally, the solvent was removed under reduced pressure
3. extractionextracted twice with DCM (500 ml)
4. washThe combined organic layers were washed with water (500 ml)
5. dry with materialdried over Na2SO4
6. customevaporated

ORD-Eintrag

ord-e984f0b46860489fa5ffafd050372951

Quelldatensatz

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07091201B2