HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → N4-(tert-butyloxycarbonyl)-N3-(4-methoxybenzoyl)-3,4-pyridinediamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | p-Anisoyl chloride | HCID 7477 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-Amino-4-(Boc-amino)pyridine | HCID 11095863 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | N4-(tert-butyloxycarbonyl)-N3-(4-methoxybenzoyl)-3,4-pyridinediamine | HCID 12069537 | 60.7% |
Reaction Steps
A solution of N4-(tert-butyloxycarbonyl)-3,4-pyridinediamine (500 mg, 2.40 mmol) and pyridine (0.213 mL, 2.63 mmol) in methylene chloride (12 mL) was treated with p-anisoyl chloride (408 mg, 2.40 mmol). After 0.75 hr, the mixture was poured into a mixture of ethyl acetate and 1 N aqueous sodium hydroxide. The organic layer was washed with saturated sodium chloride, dried (magnesium sulfate), and filtered. Concentration in vacuo and recrystallization of the residue, followed by flash chromatography (silica gel, hexanes/ethyl acetate) yielded 500 mg (60%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313151B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-cd1ac7db5bad42f69539207973a92182 |
| Source note | uspto-grants-2001_11 |