反应详情

温度

75 °C

Combine 2-(4-benzo[b]thiophen-3-yl-phenoxymethyl)-oxirane (200 mg, 0.708 mmol), 2-piperazin-1-yl-pyrimidine (465 mg, 2.83 mmol) and ethanol (4 mL). Apply heat (75° C.) to the homogeneous reaction mixtures and stir for 6 hours. Concentrate (in vacuo) and purify by column chromatography using a Waters Sep-Pak silica gel cartridge (10 g) and elution with graded solvent mixtures from 50% ethyl acetate in heptane to 100% ethyl acetate. Concentrate the appropriate fractions, dissolve in dichloromethane and re-evaporate under a stream of nitrogen. Dry the sample using medium heat and reduced pressure to give the title compound as a clear oil (0.285 mg, 90% Yield). Purity by LC/MS=99%, [M+H]+=447.

1. customto the homogeneous reaction mixtures
2. concentrationConcentrate (in vacuo)
3. custompurify by column chromatography
4. washa Waters Sep-Pak silica gel cartridge (10 g) and elution with graded solvent mixtures from 50% ethyl acetate in heptane to 100% ethyl acetate
5. concentrationConcentrate the appropriate fractions
6. dissolutiondissolve in dichloromethane
7. customre-evaporate under a stream of nitrogen
8. customDry the sample
9. temperatureusing medium heat