1,1'-Carbonyldiimidazole → HCID 22049200、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:9]([NH2:14])[C:10]([CH3:13])([OH:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8].[C:15](N1C=CN=C1)(N1C=CN=C1)=[O:16]>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([CH:9]2[C:10]([CH3:11])([CH3:13])[O:12][C:15](=[O:16])[NH:14]2)[CH:5]=[CH:6][C:7]=1[F:8]参加物
4
実験手順
A mixture of 1-(3,4-difluorophenyl)-2-methyl-2-hydroxypropylamine (3.00 g, 14.9 mmol) and carbonyldiimidazole (2.418 g, 14.9 mmol) in dichloromethane (150 mL) was heated at reflux temperature for 36 h and the solvent evaporated. The residue was purified by column chromatography on silica gel using chloroform/ethyl acetate (9:1) to give the product as a viscous oil which solidified on standing (1.80 g, 50% yield). The product was used in the next step without further characterization.
後処理
- temperaturewas heated
- temperatureat reflux temperature for 36 h
- customthe solvent evaporated
- customThe residue was purified by column chromatography on silica gel
出典と根拠
- ORDレコード
- ord-e8ff5e32a0f24432931efe60a52d3374
- 出典データセット
- uspto-grants-2006_06
- 特許番号
- US07067534B1
反応ノート
読み込み中…