反应详情

温度

80 °C

4-[6-Benzyloxy-3-[3-methoxy-4-(1-pyrrolidinylmethyl)benzyl]benzo[b]thiophen-2-yl]phenol (0.10 g; 0.19 mmol), 4-chlorobutyric acid methyl ester (27 mL; 0.22 mmol) and Cs2CO3 (0.43 g; 1.31 mmol) were combined in 2 mL of DMF and heated in an oil bath maintained at 80° C. for 3 h. After cooling to room temperature, water (30 mL) was added, and extraction was carried out with EtOAc (4×25 mL). The combined organics were washed with brine and dried by passage through Na2SO4. Purification was effected by flash chromatography on silica gel, eluting with EtOAc(100-90%)/Et3N(0-5%)/MeOH(0-5%). The title product was obtained as a colorless oil (92 mg, 78%).

1. temperatureheated in an oil bath
2. temperatureAfter cooling to room temperature
3. extractionextraction
4. washThe combined organics were washed with brine
5. dry with materialdried by passage through Na2SO4
6. customPurification
7. washeluting with EtOAc(100-90%)/Et3N(0-5%)/MeOH(0-5%)