Triphenylphosphine → HCID 11159719、化合物
反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH3:15])=[C:6]([CH:13]=1)[O:7][CH2:8][CH2:9][N:10]=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH3:15])=[C:6]([CH:13]=1)[O:7][CH2:8][CH2:9][NH2:10]参加物
5
実験手順
A solution of 2-(5-fluoro-2-methoxy-phenoxy)ethylazide (3.97 g, 0.019 mol) and triphenylphosphine (5.95 g, 0.023 mol) in tetrahydrofuran (80 ml) and water (1.5 ml) was allowed to stir for 18 hours at room temperature. The solvent was removed under vacuum. Chromatography (ethyl acetate) removed triphenylphosphine and triphenylphosphine oxide and (25-50% methanol-ethyl acetate plus ammonium hydroxide) afforded 3.14 g (90%) of product as a clear oil. MS EI m/e 185 (M+)
後処理
- customThe solvent was removed under vacuum
- customChromatography (ethyl acetate) removed triphenylphosphine and triphenylphosphine oxide and (25-50% methanol-ethyl acetate plus ammonium hydroxide)
出典と根拠
- ORDレコード
- ord-b0971bf4a1e34ebba1de9ae9005192ba
- 出典データセット
- uspto-grants-2001_09
- 特許番号
- US06291683B1
反応ノート
読み込み中…