反应详情

Pyridine-2-sulfonic acid allyl-(2,2-dimethyl-pent-4-enyl)-amide (0.6 g, 2 mmol) was diluted in CH2Cl2 (50 ml) After carefully degass by Ar, Grubbs catalyst (0.17 g, 0.2 mmol) was added under Ar protection. The mixture was then refluxed for 2 h before the solvent was removed on rotavapor. The crude product was purified by column chromatography (5%-20% E/H) to give 0.47 g of the title compound in 87% yield. MS (M+H+): 267.0; 1H-NMR (400 MHz, CDCl3): •8.70-8.69(d, 1H), 7.96-7.88(m, 2H), 7.49-7.46(m, 1H), 5.81-5.70(m, 2H), 3.93-3.92(d, 2H), 3.26(s, 2H), 2.13-2.12(d, 2H), 1.00(s, 6H)

1. additionwas added under Ar protection
2. temperatureThe mixture was then refluxed for 2 h before the solvent
3. customwas removed on rotavapor
4. customThe crude product was purified by column chromatography (5%-20% E/H)