Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Butyryl chloride | HCID 8855 | — |
| Reactant | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 2970864 | HCID 2970864 | 61.9% |
Reaction Steps
Butyryl chloride (0.53 g, 5 mmol) in dry dichloromethane (5 ml) was added dropwise with stirring to 4-piperidone ethylene ketal (0.72g, 5 mmol) and pyridine (0.5 ml) in dry dichloromethane (10 ml). The solution was stirred at 20° C. overnight then washed successively with dilute HCl, saturated sodium bicarbonate solution and water and dried (sodium sulphate). Evaporation of the solvent gave the product as a clear syrup (0.66 g). MS (+EI) 213 (M+), 1H NMR (CDCl3) 3.98 (4H, s), 3.70 (2H, t), 3.53 (2H, t), 2.33 (2H, t), 1.61-1.83 (6H, m), 0.97 (3H, t).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05883102 |
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| Source dataset | uspto-grants-1999_03 |
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| ORD ID | ord-82890ec885d441349298420957910f25 |
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| Source note | uspto-grants-1999_03 |
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