HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoromethanesulfonic anhydride → 1-Oxaspiro[4.5]decan-8-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 8-(3-Hydroxypropyl)-1,4-dioxaspiro[4.5]decan-8-ol | HCID 53866030 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Oxaspiro[4.5]decan-8-one | HCID 13298428 | — |
Reaction Steps
A mixture of 4-(3-Hydroxypropyl)-4-hydroxy-cyclohexanone ethylene ketal (1.4 g) and diisopropylethylamine (3.37 mL) in methylene chloride (100 mL) at -78° C. was treated with triflic anhydride (1.64 mL). After 30 min the reaction mixture was washed with water, the solvent was dried over magnesium sulfate and removed in vacuo. The residue was dissolved in 30 mL of tetrahydrofuran and 15 mL of 3% HCl. After 5 h at room temperature the reaction mixture was diluted with water and the product was extracted with ether. After drying over magnesium sulfate the solvent was removed in vacuo to afford 1-Oxaspiro[4.5]decan-8-one as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05585490 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-0c38a75d3224451bb57b04fd19fc9200 |
| Source note | uspto-grants-1996_12 |