Diethyl (4-fluorophenyl)phosphonate → (4-Fluorophenyl)phosphonic acid
반응식
[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]=1참가 물질
3
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-b4a9abcc4cb343e59433aa372beaa56a
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08846978B2
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