Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 178468122 | HCID 178468122 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178468121 | HCID 178468121 | — |
Reaction Steps
To a solution of 4-(ethoxy-methyl-phosphinoylmethyl)-benzoic acid methyl ester (660 mg, 2.58 mmol) in THF (5 mL) and MeOH (3 mL) was added 1N NaOH (2.58 mL, 2.58 mmol), and the mixture was stirred for 18 h. The mixture was diluted with H2O and washed with EtOAc. The aqueous layer was acidified with 1 N HCl, saturated with NaCl and extracted with a mixture of CHCl3 and MeOH, dried (MgSO4), and filtered. The solvent was evaporated under reduced pressure and the material was used without further purification. 1H NMR (CDCl3, 600 MHz) δ 7.98 (d, J=7.9 Hz, 2H), 7.34 (dd, J=7.9, 2.0 Hz, 2H), 4.12-4.03 (m, 2H), 3.26 (dd, J=25.2, 14.2 Hz, 1H), 3.23 (dd, J=25.2, 14.2 Hz, 1H), 1.44 (d, J=13.8 Hz, 3H), 1.30 (t, J=7.0 Hz, 3H). MS: cal'd 243 (MH+), exp 243 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07981874B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-166852348d4048b4a4a9271eea3b6687 |
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| Source note | uspto-grants-2011_07 |
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