Ethyl 4-[(2-amino-4-chlorophenyl)amino]-1-piperidinecarboxylate

2. Dissolve 1.34 kg of the crude product obtained in the first step in 15 liters of methanol and 15 liters of tetrahydrofuran, and add 1.3 liters. The zinc powder and 1.1 kg of ammonium chloride are reacted at 25 ° C for 5 hours, and the zinc powder is removed by filtration.The methanol and tetrahydrofuran were recovered by concentration under reduced pressure. The residue was taken up in 15 liters of ethyl acetate and washed with 15 liters of water.The organic phase was recrystallized from 1 kg of ethyl acetate and 3 kg of petroleum ether.Obtained 1.06 kg of off-white solid, domperidone intermediate (DP-2), purity 99percent, yield 88percent1.2 1-Carbethoxy-4-(2-amino-4-chloroanilino)-piperidine A solution of 59 g of 1-carbethoxy-4-(2-nitro-4-chloroanilino)-piperidine in 270 ml of tetrahydrofuran and 96 ml of absolute ethanol was hydrogenated under normal pressure and at room temperature, using 15 g of Raney nickel as a catalyst. When the uptake of hydrogen had ended, the mixture was filtered and the filtrate was evaporated. Melting point: 150° C.2. Dissolve 1.34 kg of the crude product obtained in the first step in 15 liters of methanol and 15 liters of tetrahydrofuran, and add 1.3 liters. The zinc powder and 1.1 kg of ammonium chloride are reacted at 25 ° C for 5 hours, and the zinc powder is removed by filtration.The methanol and tetrahydrofuran were recovered by concentration under reduced pressure. The residue was taken up in 15 liters of ethyl acetate and washed with 15 liters of water.The organic phase was recrystallized from 1 kg of ethyl acetate and 3 kg of petroleum ether.Obtained 1.06 kg of off-white solid, domperidone intermediate (DP-2), purity 99percent, yield 88percent1.3 1-Carbethoxy-4-(5-chlorobenzimidazol-2-on-1-yl)piperidine A mixture of 24.7 g of

Molecular Weight:297.78
XLogP3:2.7
Hydrogen Bond Donor Count:2
Hydrogen Bond Acceptor Count:4
Rotatable Bond Count:4
Exact Mass:297.1244046
Monoisotopic Mass:297.1244046
Topological Polar Surface Area:67.6
Heavy Atom Count:20
Complexity:322
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes