HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → 4'-Ethynyl-2-(trifluoromethyl)biphenyl
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2'-TrifluoroMethyl-Biphenyl-4-Carbaldehyde | HCID 1392653 | — |
| Edukt | (1E)-1-diazo-1-dimethoxyphosphorylpropan-2-one | HCID 136023029 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 4'-Ethynyl-2-(trifluoromethyl)biphenyl | HCID 86661806 | 85,4% |
Reaktionsschritte
To a stirred suspension of the product of Example 36, Step A, (0.21 g, 1 mmol) and K2CO3 (0.166 g, 1.1 mmol) in anhydrous MeOH (5 mL) was added a solution of dimethyl 1-diazo-2-oxopropylphosphonate (0.212 g, 1.1 mmol) in anhydrous MeOH (1 ml) and the mixture was stirred overnight at room temperature. The solvent was evaporated to dryness and the residue was diluted to 50 ml with EtOAc and washed with H2O. The organic layer was separated, dried over MgSO4, and filtered. The filtrate was passed through silica gel bead. The filtrate was evaporated to dryness to give the product (0.21 g, 85.4%), as creamy paste, which was used as such in next step. 1H-NMR (CDCl3) 3.11 (s, 1H); 7.25-7.31 (m, 3H); 7.44-7.55 (m, 4H); 7.73 (d, 1H, J=7.69 Hz).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09181182B2 |
| Quelldatensatz | uspto-grants-2015_11 |
| ORD ID | ord-bd7229f3ebbe4683b508cd737f42bc88 |
| Quellennotiz | uspto-grants-2015_11 |