Hydrochloric Acid → 4-Methyl-5-(2-(1-methylcyclopropyl)pyridin-4-yl)thiazol-2-amine
反応式
[CH3:1][C:2]1[N:3]=[C:4]([NH:17]C(=O)C)[S:5][C:6]=1[C:7]1[CH:12]=[CH:11][N:10]=[C:9]([C:13]2([CH3:16])[CH2:15][CH2:14]2)[CH:8]=1.Cl>CCO>[CH3:1][C:2]1[N:3]=[C:4]([NH2:17])[S:5][C:6]=1[C:7]1[CH:12]=[CH:11][N:10]=[C:9]([C:13]2([CH3:16])[CH2:15][CH2:14]2)[CH:8]=1参加物
4
実験手順
A mixture of N-{4-methyl-5-[2-(1-methyl-cyclopropyl)-pyridin-4-yl]-thiazol-2-yl}-acetamide (Step 1.3) (34.8 mmol), a 6N aqueous solution of HCl (53 mL) and EtOH (265 mL) was stirred for 5 h at 85° C., cooled to rt and then concentrated. The residue was slowly diluted with a saturated solution of NaHCO3 and then extracted with EtOAc (3×). The combined organic phases were successively washed with a saturated solution of NaHCO3 and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated with CH2Cl2 and then filtered to afford the title compound as a yellow-green solid. HPLC: t=3.55 min (method B); LC-MS: tR=1.03 min, [M+H]+ 246; TLC: Rf=0.26 (1:2 Hex/EtOAc).