Water → HCID 22000390、化合物
反応式
[CH2:1]1[CH2:8][C:7]2[CH:9]=[CH:10][C:11]([F:13])=[CH:12][C:6]=2[C:4](=[O:5])[CH2:3][CH2:2]1.[Br:14]Br.O>C(O)(=O)C>[Br:14][CH:3]1[CH2:2][CH2:1][CH2:8][C:7]2[CH:9]=[CH:10][C:11]([F:13])=[CH:12][C:6]=2[C:4]1=[O:5]参加物
5
実験手順
To a stirred solution of 8-fluoro-1-benzosuberone (20.00 g, 112.2 mmol) in glacial acetic acid (125 ml) was added bromine (5.8 ml, 112.6 mmol) dropwise. Once the addition was complete, the solution was poured into water (400 ml) and extracted with EtOAc (500 ml). The extract was separated and washed with water (500 ml). The organic layer was dried over MgSO4, filtered and evaporated to yield 100% (28.9 g) of the desired product as a viscous oil: 1H-NMR (CDCl3) δ 2.00 (2H, m), 2.33 (2H, m), 2.84 (1H, m), 3.00 (1H, m), 4.83 (1H, m), 7.13 (2H, m), 7.29 (1H, dd).
後処理
- additionOnce the addition
- extractionextracted with EtOAc (500 ml)
- customThe extract was separated
- washwashed with water (500 ml)
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-afc5ea59829f44179961c51f5856db45
- 出典データセット
- uspto-grants-2001_05
- 特許番号
- US06225330B1
反応ノート
読み込み中…