Bromine → 9-Bromomethyl-6,11-dihydro-11-oxodibenz[b,e]oxepin
反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][O:10][C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=3[C:7](=[O:16])[C:6]=2[CH:17]=1.[Br:18]Br>BrCCBr.[W]>[Br:18][CH2:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][O:10][C:9]3[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=3[C:7](=[O:16])[C:6]=2[CH:17]=1参加物
5
実験手順
To a stirred and irradiated (Tungsten lamp) solution of 2.0 gm of the 9-methyl compound of Step B in 5 ml of 1,2-dibromoethane, add a solution of 1.7 gm of bromine in 5 ml of 1,2-dibromoethane dropwise over a period of 1 hour at 150° C. Cool the reaction mixture, pour into ice water and extract with water and dry over sodium sulfate. Concentrate to dryness and crystallize the residue from isopropyl ether to obtain the title product.
後処理
- temperatureCool the reaction mixture
- extractionextract with water
- dry with materialdry over sodium sulfate
- concentrationConcentrate to dryness
- customcrystallize the residue from isopropyl ether
出典と根拠
- ORDレコード
- ord-e89b81fa23844afb95cbe6a582941ca0
- 出典データセット
- uspto-grants-1981_08
- 特許番号
- US04282365
反応ノート
読み込み中…