反应详情

温度

0 °C

To a solution of acrylic acid (34 μL, 0.49 mmol) in dichloromethane (2.4 mL) cooled at 0° C. was added 4-methylmorpholine (134 μL, 1.22 mol) and isobutyl chloroformate (74 μL, 0.57 mmol). The solution was stirred 15 minutes at 0° C. and then 4-[(4-fluorophenoxy)methyl]piperidine hydrochloride (100 mg, 0.41 mmol) was added. The mixture was stirred at room temperature overnight, diluted with water (7 mL) and extracted twice with DCM (2×5 mL). The combined organic phases were washed with water, dried over sodium sulphate and concentrated in vacuo. The residue obtained was purified by preparative TLC (eluent: dichloromethane/MeOH 95/5) to give the title compound (30 mg, 28%) as a yellow oil.

1. stirringThe mixture was stirred at room temperature overnight
2. extractionextracted twice with DCM (2×5 mL)
3. washThe combined organic phases were washed with water
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated in vacuo
6. customThe residue obtained
7. customwas purified by preparative TLC (eluent: dichloromethane/MeOH 95/5)