HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phthalic Acid → tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phthalic Acid | HCID 1017 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1-Boc-4-Methylenepiperidine | HCID 2756808 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate | HCID 22135564 | 83.6% |
Reaction Steps
13.5 g of tert-butyl 4-methylene-1-piperidinecarboxylate was dissolved in 300 ml methanol, and 28.3 g phthalic acid monoperacid magnesium salt and 8.62 g sodium bicarbonate were added thereto, and the mixture was stirred at room temperature for 1 day. The reaction solution was filtered through Celite, and the resulting filtrate was evaporated. Ethyl acetate was added to the resulting residue which was then washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and subjected to silica gel column chromatography to give 12.2 g of tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06699870B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-88932765c1a24248bf34df8e7ab3a97d |
| Source note | uspto-grants-2004_03 |