ClC1[C:10]2OC(C)C[C:6]=2[C:5]([N:12]2[C:17](=[O:18])[NH:16][C:15](=[O:19])C(C#N)=[N:13]2)=[CH:4][CH:3]=1.O1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1.[ClH:28].[C:29]([O:32]CC)(=[O:31])[CH3:30]>>[Cl:28][C:27]1[C:26]2[O:25][CH:24]([CH3:23])[CH2:10][C:6]=2[C:5]([N:12]2[C:17](=[O:18])[NH:16][C:15](=[O:19])[C:30]([C:29]([OH:32])=[O:31])=[N:13]2)=[CH:4][CH:3]=1A mixture of 9.0 g of 32C, 150 mL of p-dioxane and 100 mL of 6N hydrochloric acid was stirred at reflux temperature overnight. Then 20 mL of 12N hydrochloric acid was added and the mixture was stirred at reflux temperature for 2 hours, and stripped of solvent. The residue was dissolved in ethyl acetate, the solution was washed with water, then brine, dried (MgSO4) and stripped of solvent. The residue was recrystallized from ethyl acetate/petroleum ether to give 2-(7-chloro-2,3-dihydro-2-methyl-4-benzofuranyl)-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carboxylic acid (32D), as an amber solid, m.p.: 235°-236° C. (with decomposition).
불러오는 중…
