HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → 2-[1-(triphenylmethyl)-1H-imidazol-2-yl]acetaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Ethyl formate | HCID 8025 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2-Methyl-1-tritylimidazole | HCID 618246 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 2-[1-(triphenylmethyl)-1H-imidazol-2-yl]acetaldehyde | HCID 50990811 | — |
Reaction Steps
1.6 M of n-Butyllithium in hexane (7.5 mL) was added dropwise to a solution of 2-Methyl-1-trityl-1H-imidazole (3.244 g, 10.00 mmol) in Tetrahydrofuran (100.0 mL, 1233 mmol) at −76° C. The dark red mixture was stirred for 45 min. Ethyl formate (4.039 mL, 50.00 mmol) was added quickly and the mixture (turned yellowish) was stirred for 20 min. 6 ml of 5% aq. citric acid were added and the mixture was mixed with 60 ml of aq citric acid and extracted with ethyl acetate. The organic layer was washed with water, brine, dried over MgSO4 and concentrated in vacuum. Pale yellow semisolid material (2.025 g, 57.5%) was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09198918B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-9e59537d11e944fcbf489a5fbf29ff5d |
| Source note | uspto-grants-2015_12 |