HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 14517625, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 14517660 | HCID 14517660 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 14517625 | HCID 14517625 | — |
Reaction Steps
To a solution of 3-chloro-2-[7-fluoro-2H-1,4-benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-indazole (1.0 g) in N,N-dimethylformamide (10 ml), sodium hydride (0.3 g) and ethyl iodide (0.5 g) were successively added, and the resultant mixture was heated at 50° to 60° C., followed by stirring for 3 hours. The reaction mixture was poured into water, and the precipitated crystals were collected by filtration and purified by silica gel column chromatography using a mixture of ethyl acetate and hexane as an eluent to give Compound No. 1 (0.9 g), m.p., 101.5°-102.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04877444 |
| Source dataset | uspto-grants-1989_10 |
| ORD ID | ord-6e6097e88df64cb6b2bb551846c0827a |
| Source note | uspto-grants-1989_10 |