反应详情

温度

160 °C

A 100 mL round bottom flask containing 300 mg (0.66 mmol) of 2-(4-methoxyphenyl)benzo[b]thiophen-3-yl 4-[3-(1-pyrrolidinyl)propyl]phenyl ketone (Part A) was filled with 20 g of pyridine hydrochloride. The flask was heated to 160° C. to melt the solid. After 16 h, the reaction was cooled to warm temperature, diluted with 50 mL of H2O, and transferred to separatory funnel containing 50 mL H2O and 50 mL of EtOAc. The two layers were separated and the aqueous layer was extracted with EtOAc (2×50 mL). The combined EtOAc layers were dried over Na2SO4 and concentrated in vacuo to give 325 mg of a yellow oil. Purification by radial chromatography (SiO2; gradient of 2-10% MeOH in CH2Cl2) afforded 200 mg (0.45 mmol; 69%) of the title compound as a viscous yellow oil.

1. temperaturethe reaction was cooled
2. temperatureto warm temperature
3. customtransferred to separatory funnel
4. customThe two layers were separated
5. extractionthe aqueous layer was extracted with EtOAc (2×50 mL)
6. dry with materialThe combined EtOAc layers were dried over Na2SO4
7. concentrationconcentrated in vacuo