HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68978453, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 68978078 | HCID 68978078 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68978453 | HCID 68978453 | 73% |
Reaction Steps
8-[1-(Diphenylmethyl)azetidin-3-yl]-1,4-dioxa-8-azaspiro[4.5]decane (0.5 g, 1.4 mmol) was dissolved in dry CH2Cl2 under nitrogen and to the resultant solution was added 1-chloroethyl chloroformate (0.45 mL, 4.1 mmol) at 0° C. The mixture was stirred for 1.5 h and then methanol was added. The solution was heated to reflux for 20 min and then the solvent was removed by evaporation. The residue was triturated with acetone and the precipitate was then recrystallised from isopropyl alcohol. There was obtained 235 mg (73%) of 8-azetidin-3-yl-1,4-dioxa-8-azaspiro[4.5]decane hydrochloride as a solid. LCMS: m/z 199 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07402581B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-6eeb89053d574e14801b0f2e8391eabe |
| Source note | uspto-grants-2008_07 |