Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 54437243 | HCID 54437243 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Pentane | HCID 8003 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54081528 | HCID 54081528 | — |
Reaction Steps
The product of stage (a) above (1 g) was dissolved in dry tetrahydrofuran (20 ml) and tetramethyl ethylenediamine (1.1 ml) was added under nitrogen. The solution was cooled to -70° C. and 1.7M t-butyllithium in pentane (4.3 ml) was added dropwise. The mixture was then stirred at about -20° C. for 1 hour. It was then cooled to -70° C., and methyl iodide (0.45 g) was added. The reaction mixture was allowed to warm to 0° C. and saturated ammonium chloride solution (25 ml) was added. The mixture was extracted with tetrahydrofuran (3×50 ml) and the combined extracts were dried and evaporated to give a pale brown solid which was triturated with hexane to give 0.73 g of the desired product, mp 119°-121° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05559081 |
|---|
| Source dataset | uspto-grants-1996_09 |
|---|
| ORD ID | ord-8314191af66246a3afb38c50e15addcc |
|---|
| Source note | uspto-grants-1996_09 |
|---|