反应详情

温度

90 °C

Purge with N2 a mixture of 2-(4-bromo-2,6-dichloro-benzyl)-2-aza-spiro[4.5]decan-1-one (0.14 g, 0.36 mmol) and 4-methoxycarbonyl phenylboronic acid (0.19 g, 1.05 mmol) in toluene (10 mL) and 2M sodium carbonate (1.25 mL). Treat the reaction with Pd(PPh3)4 (0.041 g, 0.035 mmol) and heat to 90° C. for 4 hours under N2. Cool the reaction and dilute with ethyl acetate, and then wash with 1N HCl and water. Dry the organic layer with Na2SO4 and remove the solvent in vacuo to afford crude product. Purify with a 0 to 100% ethyl acetate in hexanes gradient on silica gel to afford 0.102 g (64%) of the titled product. Rf=0.51 (1/1 hexanes/ethyl acetate). MS (m/z): 446

1. customPurge with N2
2. additionTreat
3. temperatureCool
4. customthe reaction
5. washwash with 1N HCl and water
6. dry with materialDry the organic layer with Na2SO4
7. customremove the solvent in vacuo
8. customto afford crude product
9. customPurify with a 0 to 100% ethyl acetate in hexanes gradient on silica gel