Br[CH2:2][CH2:3][C:4]1([CH3:18])[CH2:9][CH2:8][C:7]2[C:10]([CH3:17])=[C:11]([OH:16])[C:12]([CH3:15])=[C:13]([CH3:14])[C:6]=2[O:5]1.[CH3:19][NH:20][CH3:21].O.[ClH:23]>CN(C)C=O.C(O)(C)C>[ClH:23].[CH3:19][N:20]([CH3:21])[CH2:2][CH2:3][C:4]1([CH3:18])[CH2:9][CH2:8][C:7]2[C:10]([CH3:17])=[C:11]([OH:16])[C:12]([CH3:15])=[C:13]([CH3:14])[C:6]=2[O:5]1
A mixture of 12.53 g of 3,4-dihydro-2-(2-bromoethyl)-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol and liquid gaseous dimethylamine in 50 ml of dimethylformamide is stirred at room temperature for 16 hours. Water is added and the product is extracted with ethyl ether. The extract is washed with water, dried over anhydrous sodium sulfate, filtered and evaporated. One equivalent of hydrochloride acid in isopropanol is added and the resulting precipitate is recrystallized twice from isopropanol/water to yield 9.44 g of the title compound, mp 300° C.
불러오는 중…
