HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 72214380, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Diethyl Carbonate | HCID 7766 | — |
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 72214380 | HCID 72214380 | — |
Reaction Steps
To a solution of lithium diisopropylamide (2M in THF/Hept/ethylbenzene, 5 mL) was added a solution of 2,4,6-collidine (1.26 mL) in THF (5 mL). The reaction mixture was stirred at RT for 4 h and added dropwise to a solution of diethylcarbonate (1.38 mL) in THF (5 mL) over 15 min. The resulting mixture was stirred at RT for 20 h. A LiOH solution (1M in water, 28 mL) was added, the mixture was stirred at RT for 2 h and filtered off. The filtrate was evaporated in vacuo. The residue was purified by preparative LC-MS (X) to afford 30 mg of yellow oil as mixture of two regioisomers. LC-MS (E): tR=0.17 min; [M+H]+: 165.97.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266876B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-37530d7146284713bff1e716fc4f3aa4 |
| Source note | uspto-grants-2016_02 |