Diethyl (4-fluorophenyl)phosphonate → (4-Fluorophenyl)phosphonic acid
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([P:8](=[O:15])([O:12]CC)[O:9]CC)=[CH:4][CH:3]=1>Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([P:8](=[O:9])([OH:15])[OH:12])=[CH:6][CH:7]=1参加物
3
実験手順
Diethyl 4-fluorophenylphosphonate (600 mg, 2.55 mmol) was combined with 8M HCl (10 mL, excess) and the mixture refluxed overnight. The reaction was cooled and filtered to remove dark specks. The solvent was removed under vacuum until a solid began to form. The mixture was then put in the refrigerator for several hours. The solid was dried to yield an off-white powder (P80 mg). 1H NMR (400.14 MHz, DMSO) δ 7.71 (ddd, J=12.49, 8.52, 5.99 Hz, 2H), 7.28 (ddd, J=9.02, 9.02, 2.65 Hz, 2H). 31P{1H} NMR (161.97 MHz, DMSO): δ 12.81. Analysis calculated (found) %: C, 40.93 (40.33), H, 3.43 (3.49).
後処理
- temperaturethe mixture refluxed overnight
- temperatureThe reaction was cooled
- filtrationfiltered
- customto remove dark specks
- customThe solvent was removed under vacuum until a solid
- customto form
- waitThe mixture was then put in the refrigerator for several hours
- customThe solid was dried
- customto yield an off-white powder (P80 mg)
出典と根拠
- ORDレコード
- ord-277c865f332b46abaee6991c20812382
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08586208B2
反応ノート
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