反应详情

温度

70 °C

A mixture of (VI) (300 mg, 1.23 mmol), N-(2-chloroethyl)morpholine hydrochloride (230 mg, 123 mmol), K2CO3 (341 mg, 2.47 mmol), and NaI (185 mg, 1.23 mmol) in dry dimethyl formamide (5 ml) was stirred overnight at 70° C. The mixture was poured into water (20 ml), extracted four times with Et2O, and the organic extracts were washed with saturated NaCl solution, dried (Na2SO4), and concentrated in vacuo. The residue was purified via MPLC (light petroleum/AcOEt 4:1) to yield (VII) (303 mg, 69%) as a colorless oil. TLC CHCl3/MeOH 9:1.

1. extractionextracted four times with Et2O
2. washthe organic extracts were washed with saturated NaCl solution
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customThe residue was purified via MPLC (light petroleum/AcOEt 4:1)