HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 2-Phenylbutane-1,2-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 2-Amino-2-phenylbutanenitrile | HCID 16794457 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Phenylbutane-1,2-diamine | HCID 21149 | 81% |
Reaction Steps
To a stirred suspension of lithium aluminum hydride (LAH, 7.0 g) in 250 mL of ether is added dropwise a solution of the compound of step 1(10.0 g) in 10 mL of ether at −70° C. The reaction mixture is stirred at −60° C. to −70° C. until TLC (10% MeOH in CH2Cl2) shows the disappearance of the starting material. The excess LAH is destroyed by cautious addition of a saturated aqueous Na2SO4 solution. The resulting mixture is filtered and solid is washed with EtOAc. The filtrate is dried over Na2SO4 and concentrated under vacuum to give 8.3 g of the title compound as clear oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06413982B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-d6ee337e164742759ca44d393570b26f |
| Source note | uspto-grants-2002_07 |