Water → Benzo-1,3-dioxole-5-carbonitrile

Temperatur

120 °C

To a solution of 3,4 Dihydroxy benzonitrile (5.0 g, 37.0 mmol) in 20 ml of DMF was added dibromomethane (19.25 g, 110.0 mmol) and potassium carbonate (25.50 g, 184.90 mmol). The reaction mixture was heated at 120° C. for 2 h under the nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), reaction mixture was cooled to room temperature. Water (50 ml) was added to the reaction mixture and extracted the compound with ethyl acetate (3×100 mL). The combined organic layers were dried over anhydrous Na2SO4, and evaporated to dryness under reduced pressure to give the title compound as yellow solid (5.16 g, 94.8%).

1. customAfter the completion of the reaction mixture (TLC monitoring), reaction mixture
2. temperaturewas cooled to room temperature
3. extractionextracted the compound with ethyl acetate (3×100 mL)
4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
5. customevaporated to dryness under reduced pressure

ORD-Eintrag

ord-dac97f44beb24917a37737a85db83b1b

Quelldatensatz

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08865736B2