HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178518988, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 12365889 | HCID 12365889 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178518988 | HCID 178518988 | — |
Reaction Steps
To a suspension of 2.44 g of 5-fluorosalicylhydroxamic acid in 22 ml of tetrahydrofuran is added 1.83 g of thionyl chloride at 10° C., and they are subjected to reaction at 20°-25° C. for one hour. Subsequently, at 10°-15° C., 4.67 g of triethylamine is dropped over 30 minutes, and thereafter, reaction is effected at 20°-25° C. for one hour. To the reaction mixture is added 200 ml of water, and the pH is adjusted to 3 with 2N hydrochloric acid. The crystals precipitated are collected by filtration to obtain 1.32 g of colorless, crystalline 5-fluoro-3-hydroxy-1,2-benzoisoxazole having a melting point of 201°-203° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05578627 |
| Source dataset | uspto-grants-1996_11 |
| ORD ID | ord-4ac0d1701a734f568cdc3ad05057c5b6 |
| Source note | uspto-grants-1996_11 |