反应详情

温度

50 °C

In a 100 ml two-neck round bottom flask 11-bromoundecanoic acid t-butyl ester (6.10 g, 19.0 mmol) was dropped into a stirred solution of NaNO2 (2.60 g, 38.0 mmol) and phloroglucinol (3.10 g, 19.0 mmol) in DMF (10 ml). The reaction mixture was warmed at 50° C. and stirred for 24 h, then poured into a mixture of 40 mL of ice/water and 40 mL of PET. After separation, the aqueous phase was further extracted with PET (3×30 mL), dried (Na2SO4) and concentrated in vacuo. The crude product was purified by silica-gel column chromatography (PET/diethyl ether 95/5) obtaining a light yellow solid (2.29 g, 42%). M.p. 39-42° C. ESI-MS: 288 (MH+); (Calc. for C15H29NO4: 287 u.m.a.).

1. customAfter separation
2. extractionthe aqueous phase was further extracted with PET (3×30 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by silica-gel column chromatography (PET/diethyl ether 95/5)