Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 86643245 | HCID 86643245 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67367219 | HCID 67367219 | — |
Reaction Steps
1-[6-(Azetidin-1-yl-methyl)-1,2,3,4-tetrahydro-isoquinolin-2-yl]-2,2,2-trifluoro-ethanone (5.162 mmol, 1 equiv.) was dissolved in methanol (20 ml); K2CO3 (10.32 mmol, 2 equiv.) was added, and the mixture was stirred for 1 hour at 25° C. Methanol was concentrated in vacuo, and the residue was taken up in dichloromethane (30 ml) and washed with distilled water (5 ml). The aqueous phase was extracted with DCM (20 ml), and the combined organic phases were dried over sodium sulfate and concentrated in vacuo. For purification, the crude product was dissolved in diethyl ether (50 ml), and a hydrochloride was precipitated with 2 M HCl in diethyl ether solution (3 equiv.). The hydrochloride was filtered off, washed with diethyl ether and dried in vacuo to yield the desired product. Yield: 1.03 g (73%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08269000B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-29444be8927343398dcb76f998c7e3da |
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| Source note | uspto-grants-2012_09 |
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