Ethylene Glycol → 2-(5-Bromo-2-methylphenyl)-1,3-dioxolane

To a solution of INT 30 (17.3 g, 87 mmol) in toluene (505 mL) was added ethane-1,2-diol (24.3 mL, 436 mmol) followed by p-toluenesulfonic acid monohydrate (0.83 g, 4.36 mmol). The reaction mixture was stirred at 130° C. for 21 hours. The mixture was washed with saturated aqueous NaHCO3 (2×) and brine (2×). The organic layer was dried over MgSO4, filtered and concentrated. The residue was purified by Kugelrohr distillation to give INT 31.

1. washThe mixture was washed with saturated aqueous NaHCO3 (2×) and brine (2×)
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. distillationThe residue was purified by Kugelrohr distillation
6. customto give INT 31

ORD-Eintrag

ord-5a0c0b5fb72943c9816dc6ef20695081

Quelldatensatz

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08791100B2