反应详情

To a solution of 3 (1.4 g, 3.3 mmol) in 20 mL of pyridine was added 0.1 g DMAP and the mixture was refluxed overnight. After removal of the pyridine, the residue was partitioned between water and ethyl acetate. The organic phase was dried, concentrated and purified by column chromatography on silica gel to afford the pure product (0.5 g, 48%) 1H NMR (400 MHz, CDCl3) δ1.44 (s, 9 H), 2.01 (m, 1 H), 3.19 (m, 1H), 3.77 (d, 3 H), 4.12 (m, 1 H), 5.08-5.16 (m, 3 H).

1. temperaturethe mixture was refluxed overnight
2. customAfter removal of the pyridine
3. customthe residue was partitioned between water and ethyl acetate
4. customThe organic phase was dried
5. concentrationconcentrated
6. custompurified by column chromatography on silica gel