HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 131723611, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22890939 | HCID 22890939 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 131723611 | HCID 131723611 | 80.9% |
Reaction Steps
To a solution of diester (viii) (86 mg, 0.18 mmol) in dioxane (1.5 mL) was added 1 N sodium hydroxide solution (720 μL, 0.72 mmol) and water (4 mL). After 3 h, the solution was neutralized and concentrated. the residue was purified by flash chromatography (elution with chloroform:methanol:concentrated ammonium hydroxide; 8.2:2:0.25) to afford the title compound (28 mg, 40%) as a colorless solid: 1H NMR (400 MHz, D2O) δH 7.84 (d, J=5 Hz, 1H, Ar—H), 7.71 (d, J=3.5 Hz, Ar—H), 7.30 (t, J=8 Hz, 1H, Ar—H), 7.15-7.21 (m, 3H, Ar—H), 7.01-7.03 (m, 1H, Ar—H), 3.23 (d, J=14 Hz, 2H, NCH2P); 31P NMR: (164 MHz, D2O) δP 14.5.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06921756B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-4604fbf6a372458283d9bb5805ebb416 |
| Source note | uspto-grants-2005_07 |