Water → HCID 59557783、化合物
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16]Br)=[CH:12][CH:11]=2)[CH:3]=1.[CH3:18][C:19]([O-:21])=[O:20].[Na+].O.C(OCC)(=O)C>CN(C=O)C>[C:19]([O:21][CH2:16][C:13]1[CH:14]=[CH:15][C:10]([CH2:9][C:4]2[CH:3]=[C:2]([Br:1])[CH:7]=[CH:6][C:5]=2[Cl:8])=[CH:11][CH:12]=1)(=[O:20])[CH3:18]参加物
6
反応条件
- 温度
- 70 °C
実験手順
To a solution of 4-bromo-2-(4-(bromomethyl)benzyl)-1-chlorobenzene (intermediate AI) (15.5 g) in DMF (70 mL), NaOAc (16.27 g) was added. The solution was heated to 70° C. After 3 h, H2O (100 mL) and ethyl acetate (200 mL) were added. The organic layer was separated, washed with brine, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AJ (8.86 g).
後処理
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over Na2SO4
- customThe solvent was evaporated under reduced pressure
- customthe product was purified by column chromatography
- customto obtain pure intermediate AJ (8.86 g)
出典と根拠
- ORDレコード
- ord-68bd2ba77fd240b3a5111cb78e4cdbf8
- 出典データセット
- uspto-grants-2010_11
- 特許番号
- US07838499B2
反応ノート
読み込み中…