HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium bisulfate → HCID 45092115, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium bisulfate | HCID 516920 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | Carbamic acid, [1-[(methoxymethylamino)carbonyl]-3-pentynyl]-, 1,1-dimethylethyl ester | HCID 21258867 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 45092115 | HCID 45092115 | — |
Reaction Steps
A suspension of lithium aluminum hydride (1.56 g, 41.1 mmol) in ether (150 mL) was stirred at room temperature for 30 minutes. The solution was cooled to -55° C. under nitrogen, and a solution of the product from Step E (11.10 g, 41.1 mmol) in ether (150 mL) was added over 15 min, maintaining the temperature below -50° C. When the addition was complete, the reaction was warmed to 5° C., then recooled to -40° C. A solution of potassium hydrogen sulfate (21.8 g) in 25 mL water was slowly added, maintaining the temperature below -35° C. The mixture was warmed to room temperature and stirred for one hour, filtered through Celite, and concentrated in vacuo to provide the title aldehyde.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05856326 |
| Source dataset | uspto-grants-1999_01 |
| ORD ID | ord-b4d9f5a00e294ca5b31e1de78e00a956 |
| Source note | uspto-grants-1999_01 |