HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diphosgene → HCID 86690139, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | HCID 86690138 | HCID 86690138 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Diisopropyl Ether | HCID 7914 | — |
| Product | HCID 86690139 | HCID 86690139 | 140.7% |
Reaction Steps
Diphosgene (0.445 ml, 3.69 mmol) was added dropwise to a stirred solution of N′-(2,2,7-trifluoro-3-oxo-4-(prop-2-ynyl)-3,4-dihydro-2H-benzo[b][1,4]oxazin-6-yl)pivalohydrazide (1311 mg, 3.69 mmol) in dry toluene (30 ml) at room temperature under nitrogen. The resulting mixture was stirred at reflux for 4 hours. It was then cooled to room temperature and evaporated in vacuo to yield 1.7 g of crude product. Trituration of this with diisopropyl ether afforded 990 mg of the title compound as a white powder (purity>95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08669208B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-506de7ec987c4124877484545941bf6c |
| Source note | uspto-grants-2014_03 |