反应详情

A mixture of cis/trans-4-(6,7-dimethoxy-quinoxalin-2-yloxy)-cyclohexanol (170 mg, 0.56 mmole) and NaH (60%, 22.4 mg, 0.56 mmole) in anhydrous THF/DMF (10 mL/2 mL) is stirred at 0° C. for 10 min. before addition of methyl iodide (50 μL, 0.56 mmole). After being stirred at ROOM TEMPERATURE for four hours, the reaction is quenched with water (0.5 mL) and concentrated. The aqueous layer is extracted with methylene chloride (2×20 mL) and the combined organic solutions are washed with brine (5 mL). The residue after concentration is chromatographed on silica gel (30% ethyl acetate/hexane) to give 80 mg (45%) of the desired product (m.p. 85-90° C.).

1. customthe reaction is quenched with water (0.5 mL)
2. concentrationconcentrated
3. extractionThe aqueous layer is extracted with methylene chloride (2×20 mL)
4. washthe combined organic solutions are washed with brine (5 mL)
5. concentrationThe residue after concentration
6. customis chromatographed on silica gel (30% ethyl acetate/hexane)