反応式
[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][NH:5][NH2:6].[Cl:8][C:9]1[C:22]2[C:21](=[O:23])[C:20]3[CH:19]=[N:18][CH:17]=[C:16]([O:24][CH2:25][C:26]4[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][CH:27]=4)[C:15]=3[C:14](=O)[C:13]=2[C:12](F)=[CH:11][CH:10]=1>N1C=CC=CC=1>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]2[N:5]([CH2:4][CH2:3][N:2]([CH3:7])[CH3:1])[N:6]=[C:14]3[C:15]4[C:16]([O:24][CH2:25][C:26]5[CH:27]=[CH:28][C:29]([O:32][CH3:33])=[CH:30][CH:31]=5)=[CH:17][N:18]=[CH:19][C:20]=4[C:21](=[O:23])[C:22]=1[C:13]=23参加物
実験手順
A solution of N-[2-(dimethylamino)ethyl]hydrazine (8.5 mg) in pyridine (0.5 mL) is added to 9-chloro-6-fluoro-4-(p-methoxybenzyloxy) benzo[g]isoquinoline-5,10-dione of Preparative Example 29 (13 mg) over a period of 2 minutes at 0° C. under a nitrogen blanket and the mixture is stirred for 2 h. The excess pyridine and some excess hydrazine are removed under a nitrogen stream. The residue is placed under vacuum overnight. The product is purified by thick layer chromathography (silica gel, 10 cm by 20 cm) using 4% methanol/96% dicloromethane. The major yellow band is scraped from the plate and the yellow compound extracted into 25% methanol/75% dicloromethane. Removal of the solvent gives 5-chloro-2-[2-(dimethylamino)ethyl]-10-(p-methoxybenzyloxy) isoquino[5,6,7-cd]indazole-6(2H)-one (3 mg) as an amorphous solid.
後処理
- customThe excess pyridine and some excess hydrazine are removed under a nitrogen stream
- customis placed under vacuum overnight
- customThe product is purified by thick layer chromathography (silica gel, 10 cm by 20 cm)
- extractionthe yellow compound extracted into 25% methanol/75% dicloromethane
- customRemoval of the solvent
出典と根拠
- ORDレコード
- ord-32bfe993475a41df8acf5a5c914ae87b
- 出典データセット
- uspto-grants-1997_01
- 特許番号
- US05596097
関連ノート
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