Dimethylformamide → HCID 58386652、化合物

反応式

C(N1[C:12]2[C:7](=[C:8]([F:14])[C:9]([F:13])=[CH:10][CH:11]=2)[CH2:6]C1=O)(=O)C.[H-].[Na+].I[CH3:19].[CH3:20][N:21]([CH:23]=[O:24])C>>[F:13][C:9]1[C:8]([F:14])=[CH:7][CH:6]=[C:20]2[C:10]=1[C:11]([CH3:12])([CH3:19])[C:23](=[O:24])[NH:21]2

参加物

反応物 4

HCID 6228Dimethylformamide

HCID 6328Methyl iodide

HCID 24758Sodium hydride

HCID 58386747HCID 58386747、化合物

生成物 1

HCID 58386652HCID 58386652、化合物

実験手順

0.50 g (2.4 mmol) 1-acetyl-4,5-difluoro-1,3-dihydro-indol-2-one were placed in 10 mL DMF under argon. 0.22 g (5.1 mmol) sodium hydride (55%) were added at 0° C. and the reaction mixture was stirred for 1 h. Then 0.32 mL (5.1 mmol) iodomethane were added dropwise. The reaction mixture was stirred overnight at RT, poured onto water and extracted with EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was purified by HPLC. The product-containing fractions were combined and concentrated to dryness by rotary evaporation.