HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9964339, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | HCID 17937804 | HCID 17937804 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9964339 | HCID 9964339 | — |
Reaction Steps
751 mg (7.0 mmol) XXII were stirred under reflux for 12 h in a mixture of 40 ml tetrahydrofuran, 20 ml water and 0.5 ml conc. H2SO4. Ethyl acetate and saturated NaCl solution were added to the reaction mixture cooled to room temperature. After separation of the phases, the aqueous phase was extracted twice with ethyl acetate and the combined organic phases were dried over Na2SO4. After column filtration (50 g SiO2, n-hexane:ethyl acetate=1:1+1% acetic acid, applied with ethyl acetate), XXIII was obtained in a yield of 448 mg (2.3 mmol, 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07060109B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-5220a8cda524421caa2c272de7d13be9 |
| Source note | uspto-grants-2006_06 |