HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Phenyl-2-pyridinamine → HCID 24995120, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Phenyl-2-pyridinamine | HCID 105097 | — |
| Reactant | 3,4-Dimethoxybenzenesulfonyl chloride | HCID 2734183 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 24995120 | HCID 24995120 | 69% |
Reaction Steps
To a solution of 5-phenylpyridin-2-amine (340 mg, 2 mmol) in 10 mL of dry pyridine was added 3,4-dimethoxybenzenesulfonyl chloride (529 mg, 2.23 mmol). The solution was stirred at room temperature under Argon. After 19 h, the pyridine was removed in vacuo and flashed off with toluene, the solid residue was partitioned between EtOAc and 1M NaOH. The alkaline phase was made acidic and the solid was collected by filtration and dried in vacuo to give 511 mg of a solid. This was taken up in 5 mL of HOAc, diluted with 3 mL of water; crystallization took place to give 447 mg of a white crystalline product with mp 202-204° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071631B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-3cf22e4b5e234afca1ed9a2a6b259c18 |
| Source note | uspto-grants-2011_12 |