HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 15171865, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Iodine chloride | HCID 24640 | — |
| Reactant | HCID 15171868 | HCID 15171868 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 15171865 | HCID 15171865 | — |
Reaction Steps
A mixture of 0.5 g (2.16 mmol) of this 4-(trifluoroacetyl)-3,4-dihydro-2H-1,4-benzoxazine, 20 ml of glacial acetic acid and 5 ml of methylene chloride was cooled to 10° in an ice bath. A solution of 1 ml of iodine monochloride in 1 ml of acetic acid was added slowly over a period of 5 minutes. Following the addition, the mixture was stirred for 45 minutes and was then diluted with water and a aqueous solution of sodium bisulfite. The product was extracted with ether. The extracts were washed with water, dried and evaporated. Crystallization of the residue from hexane yielded colorless crystals with m.p. 78°-80°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05260294 |
| Source dataset | uspto-grants-1993_11 |
| ORD ID | ord-29e03681d4c6484fa25a43154091ea16 |
| Source note | uspto-grants-1993_11 |