HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178453954, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 178501238 | HCID 178501238 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178453954 | HCID 178453954 | 69.7% |
Reaction Steps
Under argon atmosphere, a suspension of 1.29 g of lithium aluminum hydride in 40 mL of anhydrous ethyl ether was treated dropwise with a solution of 5.80 g of cis-4-(tert-butoxycarbonylamino)cyclohexanecarboxylic acid methyl ester in 20 mL of anhydrous ethyl ether with cooling in ice, and stirred for 3 hours while allowing to gradually warm to room temperature. The reaction solution was cooled to 0° C., combined a small amount of water to decompose an excessive lithium aluminum hydride. The insolubles were filtered off through Celite, and the filtrate was concentrated, and then the residue was washed with n-hexane to obtain 3.60 g of the desirable compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06794389B2 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-855e1c1293234cbb8c7483a5cb3e7514 |
| Source note | uspto-grants-2004_09 |