反应详情

145.0 g (407.9 mmol) of tert-butyl 1-[3-(benzylamino)-4-fluorobenzyl]cyclopropanecarboxylate were dissolved in 1450 ml of ethanol, and 9.67 g of palladium hydroxide (20% on carbon) were added. The suspension was stirred at RT under a hydrogen atmosphere at standard pressure for 18 h. The reaction mixture was then filtered off with suction through kieselguhr, and the filtrate was concentrated. After drying under high vacuum, 500 ml of pentane were added to the residue, resulting in the precipitation of the product. The suspension was stirred in an ice bath for 1 h. The solid was then filtered off with suction, washed twice with pentane and dried under high vacuum. 88.5 g (73.6% of theory) of the title compound were thus obtained.

1. filtrationThe reaction mixture was then filtered off with suction through kieselguhr
2. concentrationthe filtrate was concentrated
3. dry with materialAfter drying under high vacuum, 500 ml of pentane
4. additionwere added to the residue
5. customresulting in the precipitation of the product
6. stirringThe suspension was stirred in an ice bath for 1 h
7. filtrationThe solid was then filtered off with suction
8. washwashed twice with pentane
9. customdried under high vacuum