反应详情

温度

60 °C

Titanium tetraethanolate (2.70 mL, 12.9 mmol) was added to a mixture of benzyl 3-(3-acetyl-5-chloro-2-methoxy-6-methylphenyl)azetidine-1-carboxylate (2.5 g, 6.4 mmol) in 2.0 M ammonia in ethanol (16.1 mL, 32.2 mmol) at 0° C. The solution was stirred at 60° C. under N2 overnight. Sodium tetrahydroborate (0.366 g, 9.67 mmol) was added to the above mixture at 0° C. and the solution was stirred at room temperature for another 1 hour. The reaction mixture was quenched with 2 M ammonia in water and filtered. The solid was washed with acetonitrile. The solvent was removed and the residue was diluted with dichloromethane, washed with water and brine, dried over MgSO4 and concentrated to give the desired product (2.47 g, 98%). LCMS calculated for C21H26ClN2O3 (M+H)+: m/z=389.2. found: 389.1.

1. stirringthe solution was stirred at room temperature for another 1 hour
2. customThe reaction mixture was quenched with 2 M ammonia in water
3. filtrationfiltered
4. washThe solid was washed with acetonitrile
5. customThe solvent was removed
6. additionthe residue was diluted with dichloromethane
7. washwashed with water and brine
8. dry with materialdried over MgSO4
9. concentrationconcentrated