1H-Pyrrolo(2,3-b)pyridine, 2,3-dihydro-1,3,3-trimethyl-2-methylene- → HCID 15100094、化合物

反応式

[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][N:9]=2)[C:4]([CH3:12])([CH3:11])[C:3]1=[CH2:13].[N:14]([C:16]1[C:21]([O:22][CH3:23])=[CH:20][C:19]([O:24][CH3:25])=[CH:18][C:17]=1[OH:26])=O>C(O)C.CCOCC>[CH3:1][N:2]1[C:10]2=[N:9][CH:8]=[CH:7][CH:6]=[C:5]2[C:4]([CH3:11])([CH3:12])[C:3]21[CH:13]=[N:14][C:16]1[C:21]([O:22][CH3:23])=[CH:20][C:19]([O:24][CH3:25])=[CH:18][C:17]=1[O:26]2

参加物

実験手順

Into a three-necked 100 milliliter round bottom flask was charged a solution of 0.8 grams of the thus prepared 1,3,3-trimethyl-2-methylene-1,7-diazaindane in 20 milliliters of absolute ethanol. The solution was heated under a nitrogen pad to 60°-65° C. and 0.84 grams of 2-nitroso-3,5-dimethoxyphenol added to the flask. The reaction mixture was maintained at temperature and refluxing for a total reaction time of about 26 hours. The ethanol was removed on a rotary evaporator and the resulting reaction mixture taken up in ether and filtered. The ether solution sequentially was washed with 100 milliliters of a 10 percent sodium hydroxide solution, and 100 milliliters of a saturated sodium chloride solution and then dried over potassium carbonate. The ether was removed under vacuum. A silica gel column was used to isolate the final product, i.e., 1',3'-Dihydro-1',3',3'-trimethyl-5,7-dimethoxyspiro-[2H-1,4-benzoxazine-2,2'-[2H] pyrrolo[2,3-b]pyridine]. Identification of the product was confirmed by appropriate spectral analysis.