[ClH:1].[F:2][CH2:3][CH2:4][NH2:5].C(N(CC)CC)C.[Cl:13][C:14]1[CH:19]=[CH:18][C:17](C(F)(F)F)=[CH:16][C:15]=1[CH2:24][S:25](Cl)(=[O:27])=[O:26]>ClCCl>[Cl:13][C:14]1[CH:19]=[C:18]([Cl:1])[CH:17]=[CH:16][C:15]=1[CH2:24][S:25]([NH:5][CH2:4][CH2:3][F:2])(=[O:27])=[O:26]To a suspension of 2-fluoroethylamine hydrochloride (0.287 g) in dichloro-methane (4 ml) was added triethylamine (0.4 ml) followed by (2,4-dichloro-phenyl)-methanesulfonyl chloride (Example 1.2) (0.25 g). The reaction mixture was stirred at ambient temperature for 3 hours then left to stand at ambient temperature for 16 hours. Dichloromethane (20 ml) was added to the reaction mixture and the mixture was washed with water (20 ml). The phases were separated and the organic layer was dried over magnesium sulfate and concentrated to give C-(2,4-dichloro-phenyl)-N-(2-fluoro-ethyl)-methanesulfonamide (15 mg) (60% pure). 1H-NMR (400 MHz, CDCl3): 7.47-7.51 (m, 2H), 7.29-7.32 (dd, 1H), 4.77 (bs, 1H), 4.49 (s, 2H), 4.51-4.53 (m, 1H), 4.39-4.42 (m, 1H), 3.33-3.36 (m, 1H), 3.27-3.29 (m, 1H) ppm.
読み込み中…