반응 #86162

반응 방정식

tributyl-(1-tetrahydropyran-2-ylpyrazolo[4,3-c]pyridin-6-yl)stannane

2-chloro-6-methyl-pyrazine

tricyclohexylphosphine

→

6-(6-methylpyrazin-2-yl)-1-tetrahydropyran-2-yl-pyrazolo[4,3-c]pyridine

수율 64.5%

용매

N,N-Dimethylacetamide

반응 조건

후처리

1. 1
   기타The reaction mixture was sealed in a pressure vial
2. 2
   기타The mixture was partitioned between EtOAc and water
3. 3
   농축The organic layer was concentrated
4. 4
   기타the residue was purified on silica
5. 5
   세척eluted with 0 to 100% EtOAc in DCM

실험 절차

A mixture of tributyl-(1-tetrahydropyran-2-ylpyrazolo[4,3-c]pyridin-6-yl)stannane (7.139 mmol; 3514.5 mg), 2-chloro-6-methyl-pyrazine (10.71 mmol; 1377 mg), tricyclohexylphosphine; (0.5140 mmol; 144.1 mg) and tris(dibenzylideneacetone)dipalladium (0) (0.2142 mmol; 196.1 mg) in N,N-Dimethylacetamide (15 mL) was purged with Argon for 1 min. The reaction mixture was sealed in a pressure vial and heated at 130° C. overnight. The mixture was partitioned between EtOAc and water. The organic layer was concentrated and the residue was purified on silica eluted with 0 to 100% EtOAc in DCM to afford 6-(6-methylpyrazin-2-yl)-1-tetrahydropyran-2-yl-pyrazolo[4,3-c]pyridine as a clear oil (1.3608 g, 60%).

출처