HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 21060031, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | tert-Butyl 2,8-diazaspiro[4.5]decane-8-carboxylate--hydrogen chloride (1/1) | HCID 66833979 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21060031 | HCID 21060031 | 62.6% |
Reaction Steps
A stirred solution of tert-butyl 2,8-diazaspiro[4.5]decane-8-carboxylate hydrochloride (400 mg, 1.445 mmol) in DCM (5 mL) was treated with TEA (0.604 mL, 4.34 mmol), followed by Ac2O (0.164 mL, 1.734 mmol), stirred at room temperature for 2 h. To this reaction mixture was added TFA (2.115 mL, 27.5 mmol) and stirred at room temperature for h. Concentrated under reduced pressure to obtain crude material which purified by SCX cartridge, loading with MeOH, washed with additional MeOH. Product was recovered eluting with 2M NH3 in MeOH. Solvent evaporation gave 1-(2,8-diazaspiro[4.5]decan-2-yl)ethanone (165 mg)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273057B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-1d15aa6bae0344c7ba5e166c51504ed8 |
| Source note | uspto-grants-2016_03 |