Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | N,N-Dimethylethylenediamine | HCID 66053 | — |
| Reactant | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 19811356 | HCID 19811356 | 62% |
Reaction Steps
To a stirred solution of 2,4-difluoronitrobenzene (3.18 g., 20 mmole) In DMSO (5 ml) was added portion-wise N,N-dimethylethylene-diamine (3.52 g., 40 mmole). The mixture was stirred at 23° C. for 1 hour and poured into crushed ice. Ethyl acetate (200 ml) was added to dissolve the orange-yellow solid. The organic phase separated was washed with water and brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was chromatographed on a silica gel column eluting with CH2Cl2 /MeOH (20:1) to afford the compound (15) (2.8 g., 62%) which solidified on standing.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04799934 |
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| Source dataset | uspto-grants-1989_01 |
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| ORD ID | ord-e41d1517a90d406182ab963f867ac2d8 |
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| Source note | uspto-grants-1989_01 |
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