HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → cis-(+/-)-Tetrahydro-4-[[(4-methoxyphenyl)methyl]thio]-3-furanmethanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | (3R-cis)-Tetrahydro-4-[[(4-methoxyphenyl)methyl]thio]-3-furancarbonitrile | HCID 54249583 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | cis-(+/-)-Tetrahydro-4-[[(4-methoxyphenyl)methyl]thio]-3-furanmethanamine | HCID 86750347 | 99.9% |
Reaction Steps
A room temperature solution, under argon, of 4.22 ml of 1.0M lithium aluminum hydride in tetrahydrofuran is treated, dropwise, with 0.876 g of product from Example 199 in 3 ml of diethyl ether; during which time the reaction refluxes gently. After complete addition, the reaction is stirred at room temperature for 2 hour. The reaction mixture is quenched with 1 ml of water, 10.5 ml of 1.0N sodium hydroxide and 2.0 ml of water. The solid white precipitate formed is collected and washed with large volumes of diethyl ether. The diethyl ether layer is concentrated in vacuo to give 0.889 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05623081 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-6e019678e4424d6780cf162ddda63e4d |
| Source note | uspto-grants-1997_04 |