تفاعل #59065

معادلة التفاعل

1-(tert-butoxy)carbonylpiperidine-4-carboxylic acid

BOP

[4-(2-amino(4-pyridyloxy))-2-nitrophenyl]methylamine

→

tert-butyl-4-(N-{4-[4-(methylamino)-3-nitrophenoxy]-2-pyridyl}carbamoyl)piperidinecarboxylate

المذيبات

N,N-dimethyl formamide

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe resulting mixture was stirred at 60° C. for 16 h
2. 2
   تركيزThe reaction mixture was then concentrated
3. 3
   أخرىpartitioned between ethyl acetate and water
4. 4
   تجفيفThe organic layer was dried over sodium sulfate
5. 5
   أخرىthe resulting tert-butyl-4-(N-{4-[4-(methylamino)-3-nitrophenoxy]-2-pyridyl}carbamoyl) piperidinecarboxylate was purified by silica gel chromatography

الإجراء التجريبي

To a mixture of 1-(tert-butoxy)carbonylpiperidine-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 tert-butyl-4-(N-{4-[4-(methylamino)-3-nitrophenoxy]-2-pyridyl}carbamoyl) piperidinecarboxylate was purified by silica gel chromatography. MS: MH+=472.2.

المصدر