反应详情

Bis(cyclopentadienyl)zirconium chloride hydride (4.29 g, 16.27 mmol) was added portionwise over 10 min to a solution of 4-hydroxy-N-methoxy-N-methyl-3-(morpholinomethyl)benzamide (3.8 g, 13.56 mmol) in THF (50 mL), under N2 whilst maintaining the temperature below 20° C. Stirred for 2 h, quenched with saturated potassium sodium tartrate, extracted with EtOAc (3×100 mL), washed with more saturated potassium sodium tartrate and brine, dried (Na2SO4), filtered and evaporated in vacuo. Purified by flash chromatography with EtOAc as eluent to give the sub-title compound as a colourless oil. Yield: 2.1 g

1. temperaturewhilst maintaining the temperature below 20° C
2. customquenched with saturated potassium sodium tartrate
3. extractionextracted with EtOAc (3×100 mL)
4. washwashed with more saturated potassium sodium tartrate and brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo
8. customPurified by flash chromatography with EtOAc as eluent