反应详情

To a mixture of 2-cyclopropyl-methanol (6.15 g) and DMF (12 mL) was added NaH (60% in mineral oil, 1.5 g) at 0° C. After stirring for 4 hours at r.t. the mixture was diluted with DMF (5 mL) and 5-bromo-2-fluoro-pyridine (6.00 g) was slowly added keeping the reaction temperature below 30° C. After 30 minutes at r.t. the mixture was heated to 130° C. for 1 hour by microwave irradiation. After cooling to r.t. the mixture was diluted with EA and washed with water (3 times). The organic phase was dried (Na2SO4) and concentrated. The residue was purified by SGC to provide the subtitle compound. MS ESI+: m/z=228 [M+H]+.

1. additionwas slowly added
2. customthe reaction temperature below 30° C
3. temperatureAfter 30 minutes at r.t. the mixture was heated to 130° C. for 1 hour by microwave irradiation
4. temperatureAfter cooling to r.t. the mixture
5. washwashed with water (3 times)
6. dry with materialThe organic phase was dried (Na2SO4)
7. concentrationconcentrated
8. customThe residue was purified by SGC