Phosphorus tribromide → HCID 22292450、化合物
反応式
O[CH2:2][C:3]1[S:4][C:5]([S:8][CH2:9][CH2:10][CH2:11][CH3:12])=[CH:6][CH:7]=1.P(Br)(Br)[Br:14]>C(OCC)C>[Br:14][CH2:2][C:3]1[S:4][C:5]([S:8][CH2:9][CH2:10][CH2:11][CH3:12])=[CH:6][CH:7]=1参加物
4
実験手順
A solution of crude 46 (55.4 g, 0.274 mol) in anhydrous ethyl ether (70 mL) was added dropwise to a solution of phosphorus tribromide (12.9 mL, 0.137 mol) in anhydrous ethyl ether (300 mL) at 0° C. After addition was complete, the mixture was allowed to warm slowly to room temperature and stirred for 4 hours under nitrogen. The mixture was then extracted with ethyl ether (3×150 mL). The combined organic solution was washed with brine and dried (MgSO4). MgSO4 was removed by filtration and the crude product was carried to the next step without the removal of solvent to prevent product decomposition.
後処理
- additionAfter addition
- extractionThe mixture was then extracted with ethyl ether (3×150 mL)
- washThe combined organic solution was washed with brine
- dry with materialdried (MgSO4)
- customMgSO4 was removed by filtration
- customthe crude product was carried to the next step without the removal of solvent
出典と根拠
- ORDレコード
- ord-1a2e3500206c4e9e9bc656b32f0e29d9
- 出典データセット
- uspto-grants-2005_10
- 特許番号
- US06953570B2
反応ノート
読み込み中…