3-Bromo-1,1,1-trifluoro-2-propanone → HCID 67028825、化合物

反応式

[Br:1][C:2]1[C:3]([C:16](=[S:18])[NH2:17])=[CH:4][C:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[N:6][CH:7]=1.C(=O)(O)[O-].[Na+].[F:24][C:25]([F:31])([F:30])[C:26]([CH2:28]Br)=[O:27]>O1CCCC1>[Br:1][C:2]1[C:3]([C:16]2[S:18][CH2:28][C:26]([OH:27])([C:25]([F:31])([F:30])[F:24])[N:17]=2)=[CH:4][C:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:13])([CH3:14])[CH3:12])=[N:6][CH:7]=1

参加物

実験手順

To a 2 L round bottom flask was charged tert-butyl 5-bromo-4-carbamothioylpyridin-2-ylcarbamate (Intermediate 85, 50 g, 151 mmol) in tetrahydrofuran (800 mL), then solid sodium bicarbonate (25.4 g, 302 mmol) was added followed by 1,1,1-trifluoro-3-bromoacetone (31 mL, 290 mmol). The resulting mixture (yellow suspension) was allowed to stir at room temperature overnight. The white suspension was filtered and the solid was washed with water (2.2˜2.5 L). The white solid was dried under vacuum to give 56.8g of white powder (85%)