反应详情

温度

60 °C

A heterogeneous solution of Cs2CO3 (2.60 g, 4.00 mmol), NaI (30 mg, 0.20 mmol) and nonanedioic acid (0.75 g, 4.00 mmol) in THF (20 ml) was stirred for ½ hour at 60° C. Chloromethyl octanoate (1.53 g, 8.00 mmol) in THF (5 ml) was added dropwise added to the solution and stirred at 60° C. for 48 hours. The reaction mixture was cooled to room temperature and evaporated in vacuo. Diethyl ether (20 ml) was added and the residue was washed with saturated NaHCO3 (3×15 ml), dried with MgSO4 and filtered. Evaporation in vacuo gave the product as a colourless oil (0,95 g, 47.9%). 1H-NMR (CDCl3) δ 5.76 (s, 4H), 2.37 (t, 8H), 1.65 (t, 8H), 1.30 (s br, 22H), 90 (t, 6H). 13C-NMR (CDCl3) δ 172.89, 62.32, 79.44, 34.35, 34.26, 31.99, 29.32, 29.23, 29.14, 24.99, 24.86, 22.94, 14.41.

1. additionadded to the solution
2. temperatureThe reaction mixture was cooled to room temperature
3. customevaporated in vacuo
4. additionDiethyl ether (20 ml) was added
5. washthe residue was washed with saturated NaHCO3 (3×15 ml)
6. dry with materialdried with MgSO4
7. filtrationfiltered
8. customEvaporation in vacuo