HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → 5-Cyclopropyl-2,4-dinitrobenzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Cyclopropylboronic acid | HCID 2760897 | — |
| Reactant | 5-Bromo-2,4-dinitrobenzaldehyde | HCID 77231536 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 5-Cyclopropyl-2,4-dinitrobenzaldehyde | HCID 86666420 | 78% |
Reaction Steps
To a stirred solution of (iii) (3 g, 10.9 mmol) in toluene (75 mL) was added a solution of sodium carbonate (2.29 g, 21.8 mmol) in water (15 mL). The mixture was sparged with nitrogen for 10 min whereupon cyclopropyl boronic acid (1.4 g, 16.4 mmol) and tetrakis(triphenylphosphine) palladium(0) (0.25 g, 0.22 mmol) were added and the reaction mixture was heated at reflux and progress monitored by TLC. After heating for 6 h the reaction was then cooled to RT and diluted with EtOAc (100 mL). The organic layer was separated and concentrated in vacuo. Purification of the residue by column chromatography on silica gel to gave (iv) (2 g, 78%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447080B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-5fedd833e1ef4f30894f7c498eac54e6 |
| Source note | uspto-grants-2016_09 |