HRID467945

反应详情

EQUATION

反应方程式

HRID 467945 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzoic acid tert-butyl ester (Example I19) (74.14 g) in dichloromethane (750 ml) was added trifluoromethyl acetic acid (“TFA”) (148 ml). The reaction mixture was stirred at ambient temperature for 16 hours. Ethyl acetate was added and the mixture was washed with water, dried over sodium sulfate and concentrated. The residue was crystallized from ethyl acetate and heptane to give 4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-2-methyl-benzoic acid (55.0 g). 1H-NMR (CDCl3, 400 MHz): 8.12 (d, 1H), 7.65-7.45 (m, 5H), 4.15 (d, 1H), 3.75 (d, 1H), 2.75 (s, 3H).

WORKUP

后处理

  1. washthe mixture was washed with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was crystallized from ethyl acetate and heptane