Triethyl phosphite → Diethyl 3-fluorobenzylphosphonate
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5]Br.[P:10]([O:17]CC)([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13]>>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13]参加物
3
反応条件
- 温度
- 160 °C
実験手順
A mixture of 3-fluorobenzyl bromide (2 g) and triethyl phosphite (2.2 mL) was heated at 160° C. under nitrogen for 4 hours. After cooling, the were volatiles removed in vacuo and the residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100% to give diethyl (3-fluorobenzyl)phosphonate (2.46 g)
後処理
- temperatureAfter cooling
- customthe were volatiles removed in vacuo
- customthe residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100%
出典と根拠
- ORDレコード
- ord-28b00569f5bf49409286c1aa20be08a0
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09290472B2
反応ノート
読み込み中…