Methyl iodide → HCID 68455945、化合物

反応式

C(OC1C=C(C=C(OCC)C=1F)CN1CCC([NH:14][C:15](=O)[C:16]2[CH:21]=[C:20]([CH3:22])[C:19]([NH:23][CH3:24])=[N:18][CH:17]=2)CC1)C.[CH3:33][Si](C)(C)[N-][Si](C)(C)C.[Na+].CI>C1COCC1>[CH3:33][N:23]([CH3:24])[C:19]1[C:20]([CH3:22])=[CH:21][C:16]([C:15]#[N:14])=[CH:17][N:18]=1

参加物

実験手順

5-Methyl-6-methylamino-nicotinonitrile (example 121, 0.345 g, 2.34 mmol) was dissolved in 3.2 ml of abs. THF and treated at 0° C. with sodium hexamethyldisilazide-solution (1M in THF, 7.03 ml, 3.0 eq.) and, after 5 Min., 4 eq. of methyl iodide (0.58 ml). The mixture was allowed to react for 1 h at room temperature. Pouring onto crashed ice/NH4Cl, twofold extraction with AcOEt, washing with water, drying over sodium sulfate, and evaporation of the solvents, followed by flash chromatography (silica gel, hexane/AcOEt=7/3) yielded 0.330 g of the title compound as off-white solid.