反应详情

An aqueous slurry of Ni-Raney (containing 30 g of Ni on a dry basis) was washed with tetrahydrofuran, and added over a solution of 270 g (0.78 mol) of methyl 2-chloro-10-nitromethyl-10,11-dihydrodibenzo[b,f]oxepine-11-carboxylate (compound XIa), as obtained in Example 18, in 2.7 L of tetrahydrofuran. The suspension was stirred under 50-60 psi (3447-4136 hPa) of hydrogen at room temperature for 2 days. The catalyst was removed by filtration, and the resulting solution was concentrated under reduced pressure to obtain methyl 10-aminomethyl-2-chloro-10,11-dihydrodibenzo[b,f]oxepine-11-carboxylate (compound XIIa), which was used in the next step (see Example 20) without further purification.

1. washwas washed with tetrahydrofuran
2. customThe catalyst was removed by filtration
3. concentrationthe resulting solution was concentrated under reduced pressure