反应详情

To a stirred solution of compound N-[3,5-dibromo-4-[4-hydroxy-5-isopropyl-3-methylphenoxy]-2-trifluoromethyl-phenyl]malonamic acid ethyl ester of Part 11 G (15 mg, 0.027 mmol) in THF (0.5 mL) was added LiOH (0.25 mL, 1N). After 1 hour stirring the pH of reaction was adjusted to 1 by 1N HCl and the organic phase was removed in vacuo. The resulting mixture was extracted with EtOAc (3×3 mL) and the combined organic phases were dried over Na2SO4 before concentration in vacuo. The residue was purified on column (silica gel, gradient elution, CHCl3/MeOH/AcOH from 1:0:0 to 90:10:1) to give N-[3,5-dibromo-4-[4-hydroxy-5-isopropyl-3-methylphenoxy]-2-trifluoromethylphenyl]malonamic acid as a white solid (6 mg, 42%)

1. customthe pH of reaction
2. customthe organic phase was removed in vacuo
3. extractionThe resulting mixture was extracted with EtOAc (3×3 mL)
4. dry with materialthe combined organic phases were dried over Na2SO4 before concentration in vacuo
5. customThe residue was purified on column (silica gel, gradient elution, CHCl3/MeOH/AcOH from 1:0:0 to 90:10:1)