反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[F:20][C:21]1[C:26]([O:27][CH3:28])=[CH:25][CH:24]=[CH:23][C:22]=1[CH2:29]O.C(Br)(Br)(Br)[Br:32]>C(Cl)Cl>[Br:32][CH2:29][C:22]1[CH:23]=[CH:24][CH:25]=[C:26]([O:27][CH3:28])[C:21]=1[F:20]参加物
5
実験手順
Triphenylphosphine (11.1 g) was added to a solution of the subtitle product of step ii) (5.0 g) in DCM (200 ml) followed by the portionwise addition of carbon tetrabromide (14.0 g). The reaction was stirred for 4 h before the addition of further triphenylphosphine (2.0 g) and carbon tetrabromide (2.0 g) and stirring maintained for 1 h. The mixture was concentrated to 30 ml volume and diluted in Et2O (300 ml). The solid precipitate was filtered and washed with Et2O (3×) and the filtrate concentrated in vacuo. The residue was purified by column chromatography (10% Et2O/iso-hexane) to afford the subtitle compound as a clear oil. Yield: 5.2 g.
後処理
- temperaturemaintained for 1 h
- concentrationThe mixture was concentrated to 30 ml volume
- additiondiluted in Et2O (300 ml)
- filtrationThe solid precipitate was filtered
- washwashed with Et2O (3×)
- concentrationthe filtrate concentrated in vacuo
- customThe residue was purified by column chromatography (10% Et2O/iso-hexane)
出典と根拠
- ORDレコード
- ord-9f802557b38140a28afce8dfa93633d6
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07582644B2
関連ノート
読み込み中…