تفاعل #986940

ord-daeb94c8adfe457fbc462ee6103395ec

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux for 15 h
  2. 2
    تركيزconcentrated in vacuo
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (40 mL)
  4. 4
    غسيلwashed with saturated NaHCO3(aq) (30 mL)
  5. 5
    استخلاصextracted with EtOAc (4×25 mL)
  6. 6
    تجفيفThe combined organic phases were dried (MgSO4)
  7. 7
    تركيزconcentrated in vacuo

الإجراء التجريبي

A solution of 3-(1H-imidazol-4-yl)-propionic acid (1.95 g, 13.9 mmol) and H2SO4 (catalytic) in MeOH (30 mL) was heated at reflux for 15 h, then concentrated in vacuo. The residue was dissolved in CH2Cl2 (40 mL) and washed with saturated NaHCO3(aq) (30 mL). The aqueous phase was saturated with sodium chloride and extracted with EtOAc (4×25 mL). The combined organic phases were dried (MgSO4) and concentrated in vacuo to give a yellow oil (1.93 g, 90%). 1H NMR (CDCl3) δ 2.68 (t, 2H, J=7.2 Hz), 2.93 (t, 2H, J=7.2 Hz), 3.69 (s, 3H), 6.81 (s, 1H), 7.55 (s, 1H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07354934B2uspto-grants-2008_04