1-Methylpiperazine → 6-(4-Methyl-piperazin-1-yl)-benzofuran-3-one
反応式
F[C:2]1[CH:11]=[CH:10][C:5]2[C:6](=[O:9])[CH2:7][O:8][C:4]=2[CH:3]=1.[CH3:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>CS(C)=O>[CH3:12][N:13]1[CH2:18][CH2:17][N:16]([C:2]2[CH:11]=[CH:10][C:5]3[C:6](=[O:9])[CH2:7][O:8][C:4]=3[CH:3]=2)[CH2:15][CH2:14]1参加物
4
実験手順
A mixture of Example 1109B (0.152 g) and 1-methylpiperazine (0.22 g) in DMSO (1 ml) was heated at 150 C for 30 min, allowed to cool to r.t. (room temperature) then partitioned between water and EtOAc. Organics were dried (Na2SO4), concentrated and purified via silica gel chromatography eluting with 5% MeOH-CH2Cl2 to give the title compound. MS ESI(+)m/e 233.0(M+H)+.
後処理
- customthen partitioned between water and EtOAc
- dry with materialOrganics were dried (Na2SO4)
- concentrationconcentrated
- custompurified via silica gel chromatography
- washeluting with 5% MeOH-CH2Cl2
出典と根拠
- ORDレコード
- ord-fb220d5d5cb74607aea7e0751cb9882a
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07468371B2
反応ノート
読み込み中…