Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 2,2,2-Trifluoro-1-[4-(4-nitrophenyl)piperidin-1-yl]ethan-1-one | HCID 54285760 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57589953 | HCID 57589953 | — |
Reaction Steps
A solution of 1-trifluoroacetyl-4-(4-nitrophenyl)piperidine (1.42 g, 4.7 mmol) in THF (15 mL) is stirred in 25 mL 2-necked flask fitted with a condenser and pressure-equalising addition funnel. The system is flushed with N2, NaBH4 (210 mg, 5.6 mmol) is added and the flask is cooled to 0° C. A solution of iodine (600 mg, 2.3 mmol) in THF (5 mL) is then added dropwise over 20 minutes, after which the addition funnel is removed and the mixture heated at reflux overnight. The resulting pale yellow suspension is cooled to rt and MeOH (1.5 mL) is added cautiously, causing vigorous evolution of a gas. Evaporation of the solvents affords the title compound, which is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08178530B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-b841f190513548e482fc693f6ede6e3c |
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| Source note | uspto-grants-2012_05 |
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