HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 19887359, compound → HCID 19887363, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 19887359 | HCID 19887359 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Product | HCID 19887363 | HCID 19887363 | 85.7% |
Reaction Steps
12.6 g of 8-(3,3-diphenyl-2-propenyl)-4-hydroxy-4-methyl-2-oxo-3-propyl-1-oxa-3,8-diazaspiro[4,5]decane are refluxed in a mixture of 126 ml of acetic acid and 5.7 ml of acetic anhydride under nitrogen while stirring for 4 to 5 hours, then the solvent is distilled off under reduced pressure. The residue is made alkaline by adding 5% by weight aqueous sodium hydroxide solution and extracted with benzene. After washing the benzene phase with water to neutral and drying over anhydrous sodium sulfate, benzene is evaporated under reduced pressure and the remaining crude product is recrystallized from ethanol to give the title compound in 85.7% yield, m.p.: 126°-127° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05132303 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-6e85f3da00594698bf24122f0b076c66 |
| Source note | uspto-grants-1992_07 |