HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethyl phosphonoacetate → HCID 68459285, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethyl phosphonoacetate | HCID 13345 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 23070760 | HCID 23070760 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68459285 | HCID 68459285 | 102.5% |
Reaction Steps
0.038 g of sodium hydride was added to a 5 ml tetrahydrofuran solution of 0.243 g of ethyl diethylphosphonoacetate at 5° C. under a nitrogen atmosphere. 0.310 g of t-butyl 4-[1-(2-butynyl)-5-cyano-4-formyl-1H-imidazol-2-yl]piperazine-1-carboxylate dissolved in 5 ml of tetrahydrofuran was added, and the mixture was stirred for 30 minutes. 50 ml of ethyl acetate and 25 ml of 0.1N sodium hydroxide were added to the solution. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 0.380 g of the title compound was obtained from the fraction eluted with ethyl acetate-hexane (3:7).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07772226B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-28c6048fcbeb426791dd4be111f873d9 |
| Source note | uspto-grants-2010_08 |