HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Amino-1-naphthol hydrochloride → 4-(2-Chloropyridin-4-yloxy)naphthalen-1-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Amino-1-naphthol hydrochloride | HCID 2723858 | — |
| Reactant | 2-Chloro-4-fluoropyridine | HCID 2782792 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 4-(2-Chloropyridin-4-yloxy)naphthalen-1-amine | HCID 58532578 | 98.3% |
Reaction Steps
To a stirred solution of 2-chloro-4-fluoropyridine (1.261 g, 9.58 mmol) and 4-amino-1-naphthol hydrochloride (2) (750 mg, 3.83 mmol) in NMP (40 mL), at −20° C., was added potassium tert-butoxide (1.290 g, 11.50 mmol). The reaction mixture was allowed to warm to RT. After 2.5 hr, the reaction mixture was diluted with water (100 mL) and extracted with EtOAc (100 mL then 2×80 mL). The combined organic extracts were washed with brine (150 mL), dried and evaporated in vacuo. The crude product was subjected to SCX capture and release eluting with 1% NH3 in MeOH solution and the solvent was removed in vacuo to give 4-(2-chloropyridin-4-yloxy)naphthalen-1-amine (3) (1.019 g, 92%) as a brown solid: m/z 271 (M+H)+ (ES+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242960B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-42e991d8b9dc44878d87f222899e3b68 |
| Source note | uspto-grants-2016_01 |