HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphosgene → 2,6-Dichloro-3,5-dimethoxyphenyl isocyanate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | 2,6-Dichloro-3,5-dimethoxyaniline | HCID 59486253 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2,6-Dichloro-3,5-dimethoxyphenyl isocyanate | HCID 86086993 | 162% |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
A mixture of 2,6-dichloro-3,5-dimethoxy-phenylamine (500 g, 2.25 mmol), triphosgene (335 mg, 1.12 mmol) and TEA (342 g, 3.38 mmol) in dioxane (15 mL) was heated to 130° C. for 2 hours under microwave. The reaction was concentrated and the residue was purified by flash chromatography on silica eluting with DCM to obtain the title compound (450 mg, yield: 80%). 1H-NMR (400 MHz, CDCl3) δ 3.92 (s, 6H), 6.42 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434697B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-061b4f02256e4bbcbb85530fcb0c5cc2 |
| Source note | uspto-grants-2016_09 |