反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:15][CH2:16][CH2:17][CH2:18][N:19]3[CH2:23][CH2:22][CH2:21][C:20]3=[O:24])=[C:7]([N+:12]([O-])=O)[CH:8]=[N:9]2)=[CH:4][CH:3]=1.[CH3:25][O:26][CH2:27][CH2:28][C:29](Cl)=O.C(N(CC)CC)C>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]3[N:15]([CH2:16][CH2:17][CH2:18][N:19]4[CH2:23][CH2:22][CH2:21][C:20]4=[O:24])[C:29]([CH2:28][CH2:27][O:26][CH3:25])=[N:12][C:7]=3[CH:8]=[N:9][C:10]=2[CH:11]=1参加物
4
実験手順
1-[3-(7-Bromo3-nitroquinolin-4-ylamino)propyl]pyrrolidin-2-one was treated according to the methods described in Parts B, C, and D of Examples 152–156. 3-Methoxypropionyl chloride was used in Part C, and triethylamine (1.3 equivalents) was added to the reaction mixture. The crude product obtained in Part D was purified by flash chromatography on silica gel (eluting sequentially with 100:0 and 92.5:7.5 chloroform:methanol) followed by recrystallization from acetonitrile. The crystals were washed with acetonitrile and diethyl ether and dried in a vacuum oven at 60° C. to provide 1-{3-[7-bromo-2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-1-yl]propyl}pyrrolidin-2-one as a light grey solid.
後処理
- additionwas added to the reaction mixture
- customThe crude product obtained in Part D
- customwas purified by flash chromatography on silica gel (
- washeluting sequentially with 100:0 and 92.5:7.5 chloroform
- custommethanol) followed by recrystallization from acetonitrile
- washThe crystals were washed with acetonitrile and diethyl ether
- customdried in a vacuum oven at 60° C.
出典と根拠
- ORDレコード
- ord-73b5eeb65ee0473787a827af92511bab
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091214B2
関連ノート
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