تفاعل #2328

ord-ba03a2d2c49b4236818932f4fa781473

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe solid formed
  2. 2
    أخرىwas removed by filtration
  3. 3
    أخرىthe filtrate evaporated
  4. 4
    أخرىto give an oil
  5. 5
    أخرىPurification by flash chromatography on silica
  6. 6
    غسيلeluting with 0.5 to 4.0% v/v methanol/dichloromethane

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728701uspto-grants-1998_03