반응 #75721

ord-b09d54507eae4f79bde74c00241c56d9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Solvent was removed at reduced pressure
  2. 2
    workup.DISSOLUTIONthe residue dissolved in dichloromethane
  3. 3
    세척washed with 2N HCl and water
  4. 4
    건조The organic phase was dried (MgSO4) and solvent
  5. 5
    기타removed at reduced pressure

실험 절차

2-Ethyl-5-nitrobenzoic acid (0.40 g), EDC.HCl (0.45 g), cyclopropylmethylamine (0.17 g) and hydroxybenzotriazole (0.04 g) were combined in dimethylformamide (10 ml) and stirred for 18 h. Solvent was removed at reduced pressure, the residue dissolved in dichloromethane and washed with 2N HCl and water. The organic phase was dried (MgSO4) and solvent removed at reduced pressure to give the title compound (0.4 g). 1H NMR (CDCl3) δ: 0.31 (2H, m), 0.59 (2H, m), 1.09 (1H, m), 1.28(3H, t, J=7.6Hz), 2.92 (2H, m), 3.33 (2H, m), 5.97 (1H, brs), 7.45 (1H, d, J=8.4 Hz), 8.20 (2H, m).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06699879B1uspto-grants-2004_03