HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 8721397, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 28552743 | HCID 28552743 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 8721397 | HCID 8721397 | 46.2% |
Reaction Steps
A mixture of 2-amino-N-(3,4-dimethoxyphenyl)benzenesulfonamide (0.8 g, 2.6 mmol) and triphosgene (0.99 g, 3.4 mmol) in anhydrous 1,4-dioxane was heated in a sealed tube at 100° C. overnight with TLC monitoring (hexane:EtOAc, 1:1). After concentration in vacuo H2O (30 mL) was added and the mixture was extracted with EtOAc (3×100 mL). The combined organic layer was dried over Na2SO4, filtered and concentrated in vacuo. Purification by gradient flash chromatography, eluting with 20-25% EtOAc in hexane yielded the title compound (0.4 g, 1.20 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249160B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-b4fc451c1c2e448a8ce4fec04d99bac8 |
| Source note | uspto-grants-2016_02 |