Azobisisobutyronitrile → Benzoic acid, 3-(bromomethyl)-4-fluoro-, methyl ester
反応式
C1C(=O)N([Br:8])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C.[F:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][C:23]=1[CH3:32]>CCOC(C)=O>[Br:8][CH2:32][C:23]1[CH:24]=[C:25]([CH:30]=[CH:31][C:22]=1[F:21])[C:26]([O:28][CH3:29])=[O:27]参加物
5
反応条件
- 温度
- 80 °C
実験手順
NBS (14.60 g) and AIBN (2.89 g) were added to a solution of the product from step (i) (9.85 g) in EtOAc (200 mL). The resulting mixture was stirred at 80° C. for 20 h. After cooling the mixture was washed with sat. sodium thiosulphate, brine, dried, filtered and the solvent removed. The crude product was purified using chromatography, to give the subtitle compound, 5.30 g.
後処理
- temperatureAfter cooling the mixture
- washwas washed with sat. sodium thiosulphate, brine
- customdried
- filtrationfiltered
- customthe solvent removed
- customThe crude product was purified
出典と根拠
- ORDレコード
- ord-aff4b01fc1cd4aeaa683fa23fe62c11d
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08268990B2
反応ノート
読み込み中…