Dimethylformamide dimethyl acetal → HCID 68801242, 화합물
반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[N:14]([C:15]=2[C:16](=[O:18])[CH3:17])[CH:13]=[CH:12][S:11]3)=[CH:4][C:3]=1[O:19][CH3:20].CO[CH:23](OC)[N:24]([CH3:26])[CH3:25]>>[CH3:23][N:24]([CH3:26])[CH:25]=[CH:17][C:16]([C:15]1[N:14]2[C:10]([S:11][CH:12]=[CH:13]2)=[N:9][C:8]=1[C:5]1[CH:6]=[CH:7][C:2]([F:1])=[C:3]([O:19][CH3:20])[CH:4]=1)=[O:18]참가 물질
3
실험 절차
A 100 ml round bottom flask was charged with the 1-[6-(4-fluoro-3-methoxyphenyl)imidazo[2,1-b][1,3]thiazol-5-yl]ethanone (1.12 g, 3.86 mmol) and dimethylformamide dimethylacetal (25 ml). The mixture was refluxed for 20 hours and then cooled to room temperature. The mixture was concentrated in vacuo and the residue was purified by flash chromatography (ethyl acetate), giving a pale yellow solid (1.138 g, 85%). 400 MHz 1H NMR (DMSO-d6) δ: 8.39 (d, J=4.7 Hz, 1H), 7.62 (d, J=12.5 Hz, 1H), 7.45-7.40 (m, 2H), 7.31 (dd, J=11.3, 8.2 Hz, 1H), 7.20 (ddd, J=8.2, 4.3, 2.0 Hz, 1H), 5.10 (d, J=12.5 Hz, 1H), 3.87 (s, 3H), 3.06 (br. s, 3H), 2.49 (br. s, 3H). LCMS: 346 [M+H].
후처리
- temperatureThe mixture was refluxed for 20 hours
- concentrationThe mixture was concentrated in vacuo