HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 10829728, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Methyltriphenylphosphonium iodide | HCID 638159 | — |
| Reactant | Sodium 2-methylbutan-2-olate | HCID 2733478 | — |
| Reactant | HCID 10616009 | HCID 10616009 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 10829728 | HCID 10829728 | — |
Reaction Steps
A solution of sodium tert-pentoxide (70 ml of a 1M solution), prepared for immediate use, is added to a suspension of methyl(triphenyl)phosphonium iodide (25 g, 61.8 mmol) in 50 ml of toluene, and the mixture is stirred at room temperature under nitrogen for 20 minutes. The compound obtained in Step 1 (6.70 g, 20.6 mmol) dissolved in 50 ml of toluene is added dropwise and the reaction mixture is refluxed for 3 hours. After cooling, the reaction mixture is hydrolysed with a saturated NH4Cl solution and extracted with ether. The organic phase is washed with a saturated NaCl solution, H2O, dried over MgSO4 and concentrated in vacuo. The title product is purified by flash chromatography over a column (SiO2, toluene/cyclohexane:60/40).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06172097B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-a18fe4027df2428386a4ee4a5197eb1e |
| Source note | uspto-grants-2001_01 |