Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dibenzofuran | HCID 568 | — |
| Reactant | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| Reactant | Diphenyl Ether | HCID 7583 | — |
| Reactant | 3-Bromo-2,4-difluoroaniline | HCID 13732746 | — |
| Solvent | 1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) | HCID 24670 | — |
| Product | HCID 178469643 | HCID 178469643 | 78% |
Reaction Steps
A stirred mixture of 26 g of 3-amino-2,6-difluorobromobenzene and 27 g of diethyl ethoxymethylenemalonate was heated at 150° C. for 1 hour. After cooling, 100 ml of Dowtherm "A" (commercially available high boiling inert solvent mixture of diphenylether and dibenzofuran) was added and the mixture was heated under nitrogen at 260° C. for 1.5 hour. The mixture was cooled to room temperature and 200 ml of hexanes was added. The resulting precipitate was collected by filtration, washed with hexanes and dried to give a cream solid, m.p. 285° C., yield 78% (32.32 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04623650 |
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| Source dataset | uspto-grants-1986_11 |
|---|
| ORD ID | ord-f525477d456b41298c82e26a28c83bd3 |
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| Source note | uspto-grants-1986_11 |
|---|
