反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Dodecenyl succinic anhydride (179 mg, 0.67 mmol) and triethylamine (0.18 ml, 1.29 mmol) were added to a solution of compound 1 (200 mg, 0.64 mmol) in dry methylene chloride and stirred at room temperature for 2 h. The mixture was chromatographed on a silica column, and the title compound 26 was eluted from the column using 10% methanol:chloroform as eluant. The compound 26 was obtained as yellow thick syrup (352 mg, 95% yield). Rf (10:90 methanol:chloroform)=0.26. 1H NMR (300 MHz, CDCl3): δ 7.90-7.80 (m, 3H, 2C═CH, vinyl-H), 7.42-7.00 (m, 9H, Ar—H, vinyl-H), 5.30-5.05 (m, 4H), 5.00-4.95 (m, 2H), 4.82-7.78 (m, 2H), 4.65-4.40 (m, 4H), 2.85-2.70 (m, 2H), 2.50-2.40 (m, 2H), 2.30-2.10 (m, 4H), 2.08-1.90 (m, 4H), 1.90-1.70 (m, 2H), 0.91 (t, 3H, J=6.4, CH3). 13C NMR (75 MHz, CDCl3): δ 185.81, 173.27, 170.15, 161.96 (d, J=55.2), 159.45 (d, J=53.7), 135.38, 134.29, 133.30, 133.10, 131.52, 130.78, 130.51, 125.33, 124.78, 124.23 (d, J=3.1), 122.47 (d, J=13.3), 122.22 (d, J=14.8), 116.32 (d, J=18.9), 116.22 (d, J=21.8), 115.93 (d, J=25.7), 46.45 (d, J=3.2), 46.48 (d, J=3.1), 35.27, 33.08, 31.92, 29.9, 29.19, 29.44, 29.16, 28.86, 25.05, 24.21, 22.67, 14.13. ESI Mass calculated for C35H41F2NNaO4 (M+Na)+600.29. found 600.20.
WORKUP
后处理
- customThe mixture was chromatographed on a silica column
- washthe title compound 26 was eluted from the column