反应详情

The compound was prepared in the manner described by Coutts, Ian G. C.; Edwards, Mark; Richards, David J. Synthesis 1981, 487. 4-Hydroxy isophthalic acid dimethyl ester (5.28 g, 25.1 mmol) was refluxed in pyridine under a flow of N2. The reaction was monitored via TLC (20:10:1, heptane/AcOEt/AcOH) which indicated reaction completion after 8 h. The majority of the pyridine was removed under vacuum, and AcOEt (100 ml) was added. The solution was washed with 0.5 M HCl (3×50 ml). The acidic washes were then extracted with AcOEt (100 ml). The two organic phases were pooled, dried (MgSO4) and concentrated to yield a white solid (4.85 g, 99%). The solid was recrystallized from toluene (200 ml) to yield white crystals (4.6 g, 92%).

1. customThe compound was prepared in the manner
2. customSynthesis 1981, 487
3. customreaction completion after 8 h
4. customThe majority of the pyridine was removed under vacuum, and AcOEt (100 ml)
5. additionwas added
6. washThe solution was washed with 0.5 M HCl (3×50 ml)
7. extractionThe acidic washes were then extracted with AcOEt (100 ml)
8. dry with materialdried (MgSO4)
9. concentrationconcentrated