反应详情

To a suspention of 1-benzhydryl-3-ethylaminoazetidine-3-carboxylic acid amide (I-2A-1f; 36.1 g, 117 mmol) in methanol (560 ml) at room temperature was added concentrated aqueous HCl (19.5 ml, 234 mmol), resulting in a clear solution. To 20% Pd(OH)2 on carbon (3.75 g) was added methanol (85 ml), followed by the methanolic solution of I-2A-1f. The mixture was placed on a Parr® shaker and then reduced (50 psi H2) at room temperature for 20 hours. The reaction was then filtered through Celite® and then concentrated to low volume under reduced pressure, at which point a precipitate formed. The suspension was diluted with MTBE (500 ml), stirred for an additional hour, and the precipitate collected by vacuum filtration. The solid was washed washed with MTBE and then dried, in vacuo, to afford I-2A-1g (24.8 g, 98%) as a colorless solid.

1. customresulting in a clear solution
2. customat room temperature
3. customfor 20 hours
4. filtrationThe reaction was then filtered through Celite®
5. concentrationconcentrated to low volume under reduced pressure, at which point a precipitate
6. customformed
7. filtrationthe precipitate collected by vacuum filtration
8. washThe solid was washed
9. washwashed with MTBE
10. customdried, in vacuo
11. customto afford I-2A-1g (24.8 g, 98%) as a colorless solid