HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22616357, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 15480788 | HCID 15480788 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22616357 | HCID 22616357 | 97% |
Reaction Steps
To a solution of triethyl phosphonoacetate (0.72 mL, 3.6 mmol) in THF (9.4 mL) was added 60% sodium hydride (0.15 g, 3.6 mmol) under ice-cooling. The mixture was stirred at room temperature for 15 minutes, Compound 1 (0.94 g, 3.3 mmol) obtained in Example 1 was added under ice-cooling, and the mixture was stirred at room temperature for 30 minutes. Then, water was added under ice-cooling, the mixture was extracted with ethyl acetate, and the organic layer was washed with brine and dried over sodium sulfate. The solvent was evaporated in vacuo, and the residue was purified by silica gel column chromatography (eluted with hexane/ethyl acetate=2/1) to give Compound 10 (1.4 g, 97%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376535B2 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-2c96d64b638f46179eac077ef49a1d48 |
| Source note | uspto-grants-2002_04 |