Hydrogen Bromide → 4-Chloro-5-formyl-2,3,6,7-tetrahydro-1H-azepine hydrobromide
反応式
[Cl:1][C:2]1[CH2:3][CH2:4][N:5](C(OCC2C=CC=CC=2)=O)[CH2:6][CH2:7][C:8]=1[CH:9]=[O:10].[BrH:21]>C(O)(=O)C>[BrH:21].[Cl:1][C:2]1[CH2:3][CH2:4][NH:5][CH2:6][CH2:7][C:8]=1[CH:9]=[O:10]参加物
4
実験手順
10.5 gm (0.036 mol) of benzyl 4-chloro-5-formyl-2,3,6,7-tetrahydro-1H-1-azepine-carboxylate were mixed with 100 ml of a 40% solution of hydrogen bromide in glacial acetic acid, while stirring and cooling with ice. The mixture was then stirred for 3 hours at room temperature. It was then concentrated by evaporation in a rotary evaporator, and the residue was triturated with ether. After the ether had been decanted several times, the product was suction-filtered and washed twice with absolute ether.
後処理
- temperaturecooling with ice
- stirringThe mixture was then stirred for 3 hours at room temperature
- concentrationIt was then concentrated by evaporation in a rotary evaporator
- customthe residue was triturated with ether
- customAfter the ether had been decanted several times
- filtrationthe product was suction-filtered
- washwashed twice with absolute ether
出典と根拠
- ORDレコード
- ord-9eea466973144fb0a0aa34dc55483a3b
- 出典データセット
- uspto-grants-1983_11
- 特許番号
- US04414225
反応ノート
読み込み中…