HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11558955, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | HCID 58906148 | HCID 58906148 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 11558955 | HCID 11558955 | 81% |
Reaction Steps
Solution of hydroxy ketone 3 (1.64 g, 5.8 mmol) in anhydrous pyridine (12 mL) and acetic anhydride (5.5 mL) was stirred for 3 h at room temperature. It was poured into water and extracted with ethyl acetate. The organic layer was washed with saturated NaHCO3, saturated CuSO4 and water, dried (MgSO4), and evaporated to give an oily residue which was dissolved in hexane/ethyl acetate (8:2) and filtered through short path of silica gel. Evaporation of solvents gave pure crystalline acetate 4 (1.51 g, 81%). Analytical sample was obtained by recrystallization from hexane/ethyl acetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538098B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-6a435020932547d0bff95d1bbf54c313 |
| Source note | uspto-grants-2009_05 |