تفاعل #986940
ord-daeb94c8adfe457fbc462ee6103395ec
معادلة التفاعل
الكواشف
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الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةat reflux for 15 h
- 2تركيزconcentrated in vacuo
- 3workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (40 mL)
- 4غسيلwashed with saturated NaHCO3(aq) (30 mL)
- 5استخلاصextracted with EtOAc (4×25 mL)
- 6تجفيفThe combined organic phases were dried (MgSO4)
- 7تركيزconcentrated 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).