反应详情

To a mixture of PPh3 (0.26 g, 1.0 mmol) and DIAD (0.2 mL, 1.0 mmol) in dry THF (3 mL) at 0 C was added a solution of 1-(2-bromo-pyridin-3-yl)-ethanol (0.14 g, 0.67 mmol) from Step A and N-(4-p-tolyloxy-phenyl)-methanesulfonamide (0.19 g, 0.7 mmol) from Example 42 step B in dry THF (2 mL). After 1 h, the reaction was warmed to room temperature and stirred for 3 h. The reaction was then concentrated under the reduced pressure. The residue was diluted with EtOAc and the precipitates were filtered. The filtrate was brought to the usual work-up. The crude material was purified by chromatography (silica gel, 30% EtOAc/hexanes) to give the desired product. MS (EI) 413 (M+H)+.

1. concentrationThe reaction was then concentrated under the reduced pressure
2. additionThe residue was diluted with EtOAc
3. filtrationthe precipitates were filtered
4. customThe crude material was purified by chromatography (silica gel, 30% EtOAc/hexanes)