반응 #86172

반응 방정식

water

6-bromo-2-fluoro-3-methoxy-pyridine

tert-butyl N-[(3S)-3-piperidyl]carbamate

N-Methylmorpholine

→

tert-butyl N-[(3S)-1-(6-bromo-3-methoxy-2-pyridyl)-3-piperidyl]carbamate

수율 95.0%

용매

1-methyl-2-pyrrolidinone

반응 조건

후처리

1. 1
   추출extracted with EtOAc
2. 2
   농축The organic layer was concentrated
3. 3
   기타The residue was purified on silica
4. 4
   세척eluted with 0 to 40% EtOAc in Heptane

실험 절차

A mixture of 6-bromo-2-fluoro-3-methoxy-pyridine (2.030 mmol; 418.1 mg), tert-butyl N-[(3S)-3-piperidyl]carbamate (3.044 mmol; 609.7 mg), and N-Methylmorpholine (6.089 mmol; 622 mg; 0.676 mL) in 1-methyl-2-pyrrolidinone (5 mL) in a sealed pressure vial was heated at 120° C. overnight. The mixture was poured into water, and extracted with EtOAc. The organic layer was concentrated. The residue was purified on silica eluted with 0 to 40% EtOAc in Heptane to afford tert-butyl N-[(3S)-1-(6-bromo-3-methoxy-2-pyridyl)-3-piperidyl]carbamate (743.5 mg, 95%).

출처