Lithium hydroxide, monohydrate → 6-Chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylic acid
反応式
C[O:2][C:3]([C:5]1[C:13]2[O:12][N:11]=[C:10]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([CH2:21][CH3:22])=[CH:17][CH:16]=3)[C:9]=2[CH:8]=[CH:7][C:6]=1[Cl:23])=[O:4].O[Li].O>O1CCOCC1>[Cl:23][C:6]1[CH:7]=[CH:8][C:9]2[C:10]([NH:14][C:15]3[CH:16]=[CH:17][C:18]([CH2:21][CH3:22])=[CH:19][CH:20]=3)=[N:11][O:12][C:13]=2[C:5]=1[C:3]([OH:4])=[O:2]参加物
4
反応条件
- 温度
- 50 °C
実験手順
To a solution of methyl-6-chloro-3-(4-ethylphenylamino)benzo[d]isoxazole-7-carboxylate (211 mg, 638 μmol) in dioxane (10.5 ml) was added a 1N aqueous solution of LiOH hydrate (134 mg, 3190 μmol) and the resulting mixture was heated to 50° C. After 1 hr, the solvent was removed in vacuo, the residue was diluted with H2O and acidified to pH2 with 2N HCl. After diluting with EtOAc, the layers were separated and the aqueous layer was extracted with EtOAc (3×). The organics were combined, washed with brine, dried over MgSO4, filtered and concentrated to obtain the title compound as a brown solid, which was used without further purification.