HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 117874690, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 3-Butyn-2-ol | HCID 16239 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| Catalyst | Copper | HCID 23978 | — |
| Catalyst | Copper Sulfate | HCID 24462 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 117874690 | HCID 117874690 | — |
Reaction Steps
Tert-butanol (17.4 ml), water (17.4 ml), and a 1 M aqueous copper(II) sulfate solution (4.64 ml) were added to sodium chlorodifluoroacetate (3.54 g), but-3-yn-2-ol (2.00 ml), sodium azide (1.66 g), cesium carbonate (11.3 g), and copper (1.18 g), and the mixture was reacted for 30 minutes using a microwave reaction apparatus (300 W, 125° C.). The reaction solution was diluted with ethyl acetate. While being washed, the dilution was filtered to remove the aqueous layer. The organic layer was dried over anhydrous sodium sulfate and then filtered. The solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane-methyl acetate) to obtain the title compound (196 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187489B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-d47f7bbf97e446fbbc867006314bbcf4 |
| Source note | uspto-grants-2015_11 |