反应详情

The mixture of 4.90 g (16.40 mmol) of ethyl 3-(1-azetidin-3-yl-2-fluoro-2-methylpropyl)-5-fluorobenzoate, 8.17 g of 3-[bromo(4-chlorophenyl)methyl]benzonitrile, 6 mL(34.36 mmol) of DIEA in 40 mL of acetonitrile was refluxed for 4 h, then concentrated in vacuo. The mixture was poured into 150 mL of CH2Cl2 and 30 mL of aq NaHCO3. The organic layer was dried over Na2SO4 and concentrated. Two pairs of racemic compounds were separated by silica gel chromatography. Single diastereomers were separated by a chiral AD column; Mass Spectrum: m/e=523 (M+1, 35Cl), 525 (M+1, 37Cl).

1. temperaturewas refluxed for 4 h
2. concentrationconcentrated in vacuo
3. additionThe mixture was poured into 150 mL of CH2Cl2 and 30 mL of aq NaHCO3
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated
6. customTwo pairs of racemic compounds were separated by silica gel chromatography
7. customSingle diastereomers were separated by a chiral AD column