Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2H-3,1-Benzoxazine-2,4(1H)-dione, 6-nitro- | HCID 20821 | — |
| Reactant | 2-Hydroxybutanedinitrile | HCID 21253562 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178510460 | HCID 178510460 | — |
Reaction Steps
To the solution of 47.25 g of 5-nitroisatoic anhydride in 230 mL of DMF 15 g of malonitrile and 63.3 mL of triethylamine were added and the reaction mixture was stirred at 60° C. for 2 hours. The solvent was evaporated at reduced pressure and the residue was mixed with 570 mL of acetonitrile and 114 mL of concd. HCl and the solution was stirred at room temperature overnight. The precipitate was then filtered off, washed with water and ethanol to give 49.7 g of product, m.p.:>360° C. LC-MS: MH+ 231; Ret. time: 4.78 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08071601B2 |
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| Source dataset | uspto-grants-2011_12 |
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| ORD ID | ord-ae47d282d21b4cf4b96a7e291eec24aa |
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| Source note | uspto-grants-2011_12 |
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