反応式
Cl.[Cl:2][C:3]1[CH:18]=[CH:17][C:6]2[NH:7][C:8]3[S:9][C:10]([CH3:16])=[CH:11][C:12]=3[C:13]([NH2:15])=[N:14][C:5]=2[CH:4]=1.[CH3:19][O:20][CH2:21][CH2:22][C@H:23]1[CH2:28]N[CH2:26][CH2:25][NH:24]1>CS(C)=O.C1(C)C=CC=CC=1.O.C(OCC)(=O)C>[Cl:2][C:3]1[CH:18]=[CH:17][C:6]2[NH:7][C:8]3[S:9][C:10]([CH3:16])=[CH:11][C:12]=3[C:13]([N:15]3[CH2:26][CH2:25][NH:24][C@@H:23]([CH2:22][CH2:21][O:20][CH3:19])[CH2:28]3)=[N:14][C:5]=2[CH:4]=1参加物
6
反応物 2
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 130 °C
実験手順
Dissolve 7-chloro-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride (1.46 g, 4.86 mmol) and (S)-2-(2-methoxy-ethyl)-piperazine (2.1 g, 14.6 mmol) in dimethylsulfoxide/toluene (1:2)(18 ml), stir under nitrogen and heat in an oil bath at 130° C. for 28.5 hours. Stir 16 hours at ambient temperature. Dilute the mixture with water and ethyl acetate, and extract with ethyl acetate. Combine the ethyl acetate extracts, wash with water and brine, dry the organic phase (Na2SO4), filter and concentrate under reduced pressure. Chromatograph on silica gel (eluent: 0-10% 2N ammonia in methanol/dichloromethane) to give the title compound (1.14 g, 60%), Mass Spectrum (ESMS) 391/393 (M+1), mp 179-183° C. (dec).
後処理
- stirringStir 16 hours at ambient temperature
- extractionextract with ethyl acetate
- washwash with water and brine
- dry with materialdry the organic phase (Na2SO4)
- filtrationfilter
- concentrationconcentrate under reduced pressure
出典と根拠
- ORDレコード
- ord-0de79bc9bdcf4decb9130433baa099b5
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07384934B2
関連ノート
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