Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Malononitrile | HCID 8010 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 71001847 | HCID 71001847 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 71001839 | HCID 71001839 | 26% |
Reaction Steps
0.32 g (6.31 mmol) of malononitrile and 1.45 g (14.35 mmol) triethylamine were added to 2 g (6.31 mmol) of 1-ethyl-7-iodo-1H-benzo[d][1,3]oxazine-2,4-dione dissolved in 25 mL of DMF. The solution was stirred for 2 hours at 120° C. and after addition of 0.73 g (7.17 mmol) of triethylamine, for another 1 hour at 110° C. The DMF was then evaporated under reduced pressure and the residue taken over with a mixture of water and dichloromethane. Filtration of this mixture gave a first fraction of the expected compound: 0.55 g (1.62 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09126972B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-18bd85c1152f4ff594657229cfe8ef5e |
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| Source note | uspto-grants-2015_09 |
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