Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate → ((1-Ethyl)(4-piperidyl))-n-{4-{4-(methylamino)-3-nitrophenoxy}(2-pyridyl)}carboxamide

To a mixture of 1-(ethyl)piperidine-4-carboxylic acid (1 eq) in N,N-dimethyl formamide and N,N-disopropylethylamine (4 eq) was added BOP (2 eq) and the mixture was stirred at ambient temperature until homogeneous. To it was added [4-(2-amino(4-pyridyloxy))-2-nitrophenyl]methylamine (1 eq) and the resulting mixture was stirred at 60° C. for 16 h. The reaction mixture was then concentrated and partitioned between ethyl acetate and water. The organic layer was dried over sodium sulfate and the resulting ((1-ethyl)(4-piperidyl))-N-{4-[4-(methylamino)-3-nitrophenoxy]}(2-pyridyl))carboxamide was purified by silica gel chromatography. MS: MH+=400.2.

1. stirringthe resulting mixture was stirred at 60° C. for 16 h
2. concentrationThe reaction mixture was then concentrated
3. custompartitioned between ethyl acetate and water
4. dry with materialThe organic layer was dried over sodium sulfate
5. customthe resulting ((1-ethyl)(4-piperidyl))-N-{4-[4-(methylamino)-3-nitrophenoxy]}(2-pyridyl))carboxamide was purified by silica gel chromatography

ORDレコード

ord-95dc3978bdd54c49b4a98563105ed856

出典データセット

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08415382B2