반응 #2328

반응 방정식

Methyl 4-(2,2-dimethylbromoacetyl)phenoxyacetate

1-(4-pyridyl)piperazine

→

title compound

Methyl 4-[2-[4-(4-pyridyl)piperazin-1-yl]-2,2-dimethyl-acetyl]phenoxyacetate

용매

acetonitrile

반응 조건

후처리

1. 1
   기타the solid formed
2. 2
   기타was removed by filtration
3. 3
   기타the filtrate evaporated
4. 4
   기타to give an oil
5. 5
   기타Purification by flash chromatography on silica
6. 6
   세척eluting with 0.5 to 4.0% v/v methanol/dichloromethane

실험 절차

Methyl 4-(2,2-dimethylbromoacetyl)phenoxyacetate (1.58 g) was added to a stirred solution of 1-(4-pyridyl)piperazine (1.63 g) in acetonitrile (40 ml). After 34 days, the solid formed was removed by filtration and the filtrate evaporated to give an oil. Purification by flash chromatography on silica, eluting with 0.5 to 4.0% v/v methanol/dichloromethane gave the title compound, 240 mg, as a white foam: NMR (d6DMSO) δ 8.49 (2H, d), 8.12 (2H, d), 6.96 (2H, d), 6.77 (2H, d), 4.87 (2H, s), 3.69 (3H, s), 3.28 (4H, t), 2.58 (4H, t), 1.25 (6H, s); m/e 398 (M+H)+ ; calculated for C22H27N3O4.0.25H2O: C, 65.7; H, 6.8; N, 10.4. found: C, 65.3; H, 6.9; N, 10.4%.

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