HRID2427875

反应详情

EQUATION

反应方程式

HRID 2427875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-[2-(4-fluoro-phenyl)-6-(4-trifluoromethyl-phenyl)-pyridin-4-yl]-4-methyl-pentanoic acid methyl ester (80 mg, 0.18 mmol) in NaOH (1N, 1 mL) and THF (4 mL) was stirred at 40° C. overnight. The mixture was cooled to room temperature, acidified with 10% citric acid, and extracted with CH2Cl2 (3×). The organic layer was washed with brine, dried over Na2SO4, filtered and evaporated. The residue was purified by chromatography (5-25% ethyl acetate in CH2Cl2) to give the product as a white foam (60 mg, 77%). 1H NMR (300 MHz, CDCl3) δ 8.21 (d, J=8.29 Hz, 2H), 8.05-8.15 (m, 2H), 7.73 (d, J=8.29 Hz, 2H), 7.65 (d, J=1.51 Hz, 2H), 7.11-7.23 (m, 2H), 3.80 (t, J=7.72 Hz, 1H), 2.08-2.16 (m, 1H), 1.77 (dt, J=7.06, 13.75 Hz, 1H), 1.48-1.64 (m, 1H), 0.96 (d, J=6.40 Hz, 6H). MS m/e 432.3 (M+H).

WORKUP

后处理

  1. extractionextracted with CH2Cl2 (3×)
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by chromatography (5-25% ethyl acetate in CH2Cl2)