HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → (2,4-Difluoro-3-formyl-phenyl)-carbamic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Reactant | Tert-butyl (2,4-difluorophenyl)carbamate | HCID 22986665 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (2,4-Difluoro-3-formyl-phenyl)-carbamic acid tert-butyl ester | HCID 58086596 | — |
Reaction Steps
To 2,4-difluoro-phenyl)-carbamic acid tert-butyl ester (123, 1.41 g, 6.17 mmol) in tetrahydrofuran (60.0 mL) under an atmosphere of nitrogen at 78° C. were added n-butyllithium (2.50 M in hexane, 2.59 mL) for 30 min. Lithium diisopropylamide (2.0 M in hexane, 3.4 mL) was added to the reaction. After 35 min, N,N-dimethylformamide (1.05 mL, 0.0136 mol) was added to the reaction mixture. The reaction was allowed to cool to room temperature overnight. The organic layer was washed with brine, dried over sodium sulfate, concentrated and purified by silica gel chromatography, eluting with 20% ethyl acetate in hexane to provide compound 124.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415469B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-b818de35d6b3485f9327345dcd56453a |
| Source note | uspto-grants-2013_04 |