HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-2-fluoroaniline → 4-(4-Chloro-2-fluoro-phenylamino)-7-(3-chloro-propoxy)-6-methoxy-quinoline-3-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-2-fluoroaniline | HCID 93898 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Pyridinium chloride | HCID 10176127 | — |
| Reactant | 4-Chloro-7-(3-chloropropoxy)-6-methoxyquinoline-3-carbonitrile | HCID 11220637 | — |
| Solvent | Glycol monoethyl ether | HCID 8076 | — |
| Product | 4-(4-Chloro-2-fluoro-phenylamino)-7-(3-chloro-propoxy)-6-methoxy-quinoline-3-carbonitrile | HCID 10202274 | 68.8% |
Reaction Steps
A mixture of 3.1 g (9.96 mmol) of 7-(3-Chloro-propoxy)-4-chloro-6-methoxy-quinoline-3-carbonitrile, 1.6 g (10.96 mmol) of 4-chloro-2-fluoro-aniline, and 1.2 g (10 mmol) of pyridine hydrochloride in 31 ml of 2-ethoxyethanol was stirred at reflux for 1.5 hr. The mixture was poured into saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic solution was dried and solvent was removed. The residue was purified on a silica gel column eluting with chloroform-ether mixtures to give 2.88 g of the title compound as an off-white solid powder: mass spectrum (electrospray, m/e) M+H 419.7.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06002008 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-67b9bfde143d463698e74e117208e398 |
| Source note | uspto-grants-1999_12 |