反应详情

Methyl1-[(cyclopentylamino)methyl]cyclopentane-1-carboxylate (Intermediate 258; 1.60 g, 7.10 mmol), 2,4-dichloro-5-nitropyrimidine (Aldrich; 1.66 g, 8.52 mmol) and triethylamine (1.2 mL, 8.52 mmol) were stirred in acetonitrile (50 mL) for 4 hours. The reaction mixture was evaporated and the residue dissolved in DCM, washed with water, dried (MgSO4) and evaporated. The residue was purified on a silica column eluting with 1% methanol/DCM to yield the title compound as a yellow oil that crystallised on standing (945 mg, 35%).

1. customThe reaction mixture was evaporated
2. dissolutionthe residue dissolved in DCM
3. washwashed with water
4. dry with materialdried (MgSO4)
5. customevaporated
6. customThe residue was purified on a silica column
7. washeluting with 1% methanol/DCM