反应详情

A mixture of 4-[4-(phenylmethyl)-1-piperazinyl]-benzoic acid (0.0145 mol), O-(tetrahydro-2H-pyran-2-yl)-hydroxylamine (0.029 mol), N,N-methanetetrayl-biscyclohexanamine (0.0145 mol) and 1-hydroxy-1H-benzotriazole (0.021 mol) in DCM p.a. (200 ml) was stirred at room temperature over the weekend. The reaction mixture was washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from EtOAc, filtered off and dried, yielding 3.5 g and another crop: 2.0 g total yielding 5.5 g (95%) of 4-[4-(phenylmethyl)-1-piperazinyl]-N-[(tetrahydro-2H-pyran-2-yl)oxy]-benzamide (interm. 8).

1. washThe reaction mixture was washed with water
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. customthe solvent was evaporated
5. customThe residue was crystallized from EtOAc
6. filtrationfiltered off
7. customdried
8. customyielding 3.5 g