HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 90302550, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 90302644 | HCID 90302644 | — |
| Reactant | HCID 90302656 | HCID 90302656 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 90302550 | HCID 90302550 | — |
Reaction Steps
Hexyl 4-(phenylcarbamoyl)thiophene-3-carboxylate (4) (0.2949 g, 0.000890 mol), hexyl 2,5-dibromo-4-(phenylcarbamoyl)thiophene-3-carboxylate (7) (0.2952 g, 0.000890 mol), palladium catalyst (4% mol), ligand (8% mol) and Cs2CO3 (162.9 mg; 0.50 mmol) were put in a microwave vial with a magnetic stirring bar. Tetrahydrofuran (1 mL) was added and sealed. 5 cycles of freeze pump thaw was done and the reaction was kept at 120 degree Celsius for 48 hours. The whole mixture was cooled to room temperature and poured in 500 mL of cold methanol. The precipitate was filtered and dissolved in THF and precipitated again. This procedure was repeated 3 times to remove small molecules.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09355787B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-5195d90d83394261b46cf2954f2730da |
| Source note | uspto-grants-2016_05 |