HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorotrimethylsilane → ((Dihydrofuran-2(3H)-ylidene)(methoxy)-methoxy)trimethylsilane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | Methyl tetrahydrofuran-2-carboxylate | HCID 169922 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | ((Dihydrofuran-2(3H)-ylidene)(methoxy)-methoxy)trimethylsilane | HCID 67099887 | — |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
To a suspension of LDA (2.6 g, 24.3 mmol) in THF (30 mL) at −78° C. was slowly added methyl tetrahydrofuran-2-carboxylate (3.0 g, 23.0 mmol). The resulting mixture was stirred at −78° C. for 20 minutes, and TMS chloride (2.6 g, 24.3 mmol) was slowly added. The reaction was stirred for 1 hour at −78° C. and then warmed to room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure, avoiding contact with water. Hexanes (20 mL) was then added, and the mixture was passed through a short plug of celite, eluting with hexanes (10 mL). The solution was then concentrated, affording the crude product in good purity.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928139B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-c7776747b56d4a5098e3e1e9b3059cff |
| Source note | uspto-grants-2011_04 |