HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 178527357, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | 18-Crown-6 | HCID 28557 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | 5-Bromo-2-[(4-fluorobenzene-1-sulfonyl)methyl]aniline | HCID 58656513 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 178527357 | HCID 178527357 | — |
Reaction Steps
To a suspension of (5-bromo-2-{[(4-fluorophenyl)sulfonyl]methyl}phenyl)amine (Intermediate 68) (0.42 g) in chloroform (10 ml) was added potassium acetate (0.135 g) and acetic anhydride (0.24 ml). The mixture was heated under nitrogen at reflux for 18 h. 18-Crown-6 (0.64 g) and tert-butylnitrite (0.435 ml) were added and the mixture was stirred at reflux for a further 42 h. The mixture was concentrated under vacuum and the residue was purified by column chromatography on silica eluting with cyclohexane:ethylacetate (4:1) to give the title compound (0.16 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07642276B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-5ec11b7628b4469aa5e6f7f5dca8e6d8 |
| Source note | uspto-grants-2010_01 |