反应详情

N-[3,5-Dichloro-4-(4-hydroxy-3-nonylcarbamoyl-phenoxy)-phenyl]-malonamic acid methyl ester (78 mg, 0.14 mmol) was dissolved in a mixture of MeOH (2 ml), water (1.5 ml), and 1 M NaOH (0.5 ml, 0.5 mmol). The resulting solution was stirred at RT for 2 h then diluted with 15 ml 0.1 M KOH. The solution was washed with a 1:1 mixture of Et2O and EtOAc (3×10 ml) and the combined organic washings were extracted with 0.1 M KOH (2×10 ml). The combined basic solutions were acidified with concentrated HCl and extracted with EtOAc (3×15 ml) and the combined organic extracts washed with brine. The dried extracts were filtered and concentrated to give the title compound of Step G and Example 3, (64 mg). MS (APCI+) Calc.: 524.1, Found: 525.1 (M+).

1. washThe solution was washed with a 1:1 mixture of Et2O and EtOAc (3×10 ml)
2. extractionthe combined organic washings were extracted with 0.1 M KOH (2×10 ml)
3. extractionextracted with EtOAc (3×15 ml)
4. washthe combined organic extracts washed with brine
5. filtrationThe dried extracts were filtered
6. concentrationconcentrated