Sulfuric Acid → 3-Cyclopropylamino-2-methyl-4-(methylsulfonyl)benzoic acid
반응식
F[C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[S:11]([CH3:14])(=[O:13])=[O:12])[C:5]([OH:7])=[O:6].[CH:16]1([NH2:19])[CH2:18][CH2:17]1.S(=O)(=O)(O)O>>[CH:16]1([NH:19][C:2]2[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=2[S:11]([CH3:14])(=[O:13])=[O:12])[C:5]([OH:7])=[O:6])[CH2:18][CH2:17]1참가 물질
4
반응 조건
- 온도
- 120 °C
실험 절차
5.0 g (22 mmol) of 3-fluoro-2-methyl-4-(methylsulfonyl)benzoic acid were dissolved in 25.0 ml (356 mmol) of cyclopropylamine. With stirring, the mixture was then heated in an autoclave at 120° C. for 1 day, and then cooled to room temperature (RT), acidified with a mixture of ice-water and conc. sulfuric acid and extracted with ethyl acetate. The combined organic phases were dried over MgSO4, and the solvent was removed under reduced pressure. The residue was purified by preparative HPLC. This gave 1.8 g of a beige solid of purity of 95%.