Cl.O1[C:6]2([CH2:11][CH2:10][CH:9]([NH:12][C:13]3[N:18]=[C:17]([N:19]4[C:27]5[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=5)[CH:21]=[N:20]4)[CH:16]=[CH:15][N:14]=3)[CH2:8][CH2:7]2)[O:5]CC1.[OH-].[Na+]>C1COCC1>[N:19]1([C:17]2[CH:16]=[CH:15][N:14]=[C:13]([NH:12][CH:9]3[CH2:8][CH2:7][C:6](=[O:5])[CH2:11][CH2:10]3)[N:18]=2)[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[N:20]1Aqueous HCl (3 M, 40 mL) was added to (1,4-dioxaspiro[4.5]dec-8-yl)-(4-indazol-1-yl-pyrimidin-2-yl)-amine (1.89 g, 5 mmol) in THF (40 mL), and the resulting mixture heated to 80° C. for 1 h. The reaction mixture was cooled and poured onto a mixture of ice and aqueous NaOH (1 M, 120 mL), and the resulting suspension filtered. The collected solids were washed with water, taken up in DCM/MeOH, and a portion of the solvent evaporated under reduced pressure. The resulting suspension was filtered, the collected solids washed with hexanes, and dried under reduced pressure to give 4-(4-indazol-1-ylpyrimidin-2-ylamino)-cyclohexanone (1.57 g, 95% yield) as a white powder. MS=308 [M+H]+; MP=211.8-213.2° C.
読み込み中…