HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diphosgene → 5-Isocyanato-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | 5-Amino-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 54171543 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 5-Isocyanato-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 18995941 | 84.2% |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
37 g of the product of Example 33 were dissolved in 50 ml of absolute 1,4-dioxane, and a solution of 13.5 g of diphosgene in 80 ml of absolute 1,4-dioxane was added. The mixture was then stirred for 6 hours at 110° C. (bath temperature), the solvent was then removed under vacuum and the remaining residue was subjected to fractional distillation under vacuum to give 18 g of product (=44% of theory) with a boiling point of 63° C. at 0.1 mbar. NMR: -59.3 and -85.0 ppm. 1H NMR: 3.0 ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05420309 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-736b9ea5027648c8a3746f1d33760ede |
| Source note | uspto-grants-1995_05 |