反应详情

Mix (2-benzothiazolyl)(4-piperidinyl)methanone.CF3CO2H (331 g, 9.19 mmol), 2-(4-methoxyphenyl)ethyl bromide (2.07 g, 9.64 mmol), potassium carbonate (3.33 g, 24.1 mmol) and dimethylformamide (35 mL) and heat at 90° C. overnight. Cool to room temperature and partition between a 2:1 mixture of ethyl acetate/toluene and water. Separate the aqueous phase and wash the organic phase with water and brine. Dry (MgSO4) and evaporate the solvent in vacuo. Purify by chromatography (30% ethyl acetate/hexane) and recrystallize (cyclohexane) to give the title compound as a tan powder; mp 119°-120° C.

1. custompartition between a 2:1 mixture of ethyl acetate/toluene and water
2. customSeparate the aqueous phase
3. washwash the organic phase with water and brine
4. dry with materialDry (MgSO4)
5. customevaporate the solvent in vacuo
6. customPurify by chromatography (30% ethyl acetate/hexane)
7. customrecrystallize (cyclohexane)