Dichloromethane → 1,3-Benzodioxole, 5-methyl-

Temperatur

100 °C

A mixture of 4-methylcatechol (26.0 g, 209.4 mmol) and NaOH (18.4 g, 461.0 mmol) in CH2Cl2 (40.0 mL) was heated to 100° C. under nitrogen for 2 hours. The solution was allowed to cool to ambient temperature and diluted with ethyl acetate (500 mL). The mixture was washed with NaHCO3 (200 mL) and H2O (2×200 mL). The organic layer was dried over Na2SO4, filtered and concentrated to give a crude oil. Flash chromatography eluting with hexane (100%) gradient to ether/hexane (1:1) afforded the title intermediate as a colorless oil 20.5 g (71.9%).

1. temperatureto cool to ambient temperature
2. washThe mixture was washed with NaHCO3 (200 mL) and H2O (2×200 mL)
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto give a crude oil
7. washFlash chromatography eluting with hexane (100%) gradient to ether/hexane (1:1)

ORD-Eintrag

ord-07f0cc7de98e4b4aa8fd7d1923e436ad

Quelldatensatz

uspto-grants-2003_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06605596B2