반응 #2129022

반응 방정식

Diethyl 4-fluorophenylphosphonate

→

4-fluorophenylphosphonic acid

용매

HCl

반응 조건

후처리

1. 1
   온도the mixture refluxed overnight
2. 2
   온도The reaction was cooled
3. 3
   여과filtered
4. 4
   기타to remove dark specks
5. 5
   기타The solvent was removed under vacuum until a solid
6. 6
   기타to form
7. 7
   workup.WAITThe mixture was then put in the refrigerator for several hours
8. 8
   기타The solid was dried
9. 9
   기타to yield an off-white powder (P80 mg)

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).

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