HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Fluoride → 2-Amino-3-nitro-5-propenyl-benzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | Methyl 2-amino-5-bromo-3-nitrobenzoate | HCID 17984898 | — |
| Reactant | Stannane, tributyl-1-propenyl- | HCID 57369809 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2-Amino-3-nitro-5-propenyl-benzoic acid methyl ester | HCID 66940429 | 77% |
Reaction Steps
A solution of 0.5 g (1.8 mmol) of the above ester 0.9 g (2.7 mmol) of tributyl-propenyl-stannane, 0.18 g (0.18 mmol) of (tetrakistriphenyl phosphine) palladium (0) in 25 mL of dioxane was degassed with nitrogen for 20 min then refluxed under nitrogen for 12 h. The reaction mixture was cooled, 20 mL of 2 M KF solution was added. The mixture was stirred for 20 min, extracted with ethyl acetate washed with water and brine. The residue was purified by column chromatography using 8:2 hexane and ethyl acetate to afford 0.35 g (77%) of the 2-amino-3-nitro-5-propenyl-benzoic acid methyl ester as a solid LCMS: 239 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07893267B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-cc70be09795b476180a4cabd9005a3ff |
| Source note | uspto-grants-2011_02 |