HRID1963701

反应详情

EQUATION

反应方程式

HRID 1963701 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  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