HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Diethoxyphosphorylpropan-2-one → HCID 59684847, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Diethoxyphosphorylpropan-2-one | HCID 14028 | — |
| Reactant | (3-Trifluoromethylphenyl)urea | HCID 25712 | — |
| Reactant | 4-Cyanobenzaldehyde | HCID 66042 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59684847 | HCID 59684847 | — |
Reaction Steps
A solution of diethyl (2-oxopropyl)phosphonate (250 mg, 1.29 mmol), 4-cyanobenzaldehyde (168.84 mg, 1.29 mmol), N-[3-(trifluoromethyl)phenyl]urea (263 mg, 1.29 mmol) and polyphosphoric acid ethyl ester (0.70 g) in tetrahydrofuran (5 ml) is refluxed overnight with stirring. The reaction solution is purified directly by preparative HPLC (RP18 column; eluent: acetonitrile/water 10:90→90:10). The fractions containing product are concentrated in vacuo and re-purified by flash chromatography on silica gel 60 with dichloromethane/methanol as eluent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101615B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-b840854984ea4689811308eac39eb028 |
| Source note | uspto-grants-2012_01 |