Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 18723402 | HCID 18723402 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18723226 | HCID 18723226 | — |
Reaction Steps
19.21 kg of tert-butyl 4-(4-trifluoromethoxybenzyloxy)piperidin-1-carboxylate and 50 L of ethanol were mixed, and stirred at 60° C. The mixture was mixed with 8.28 L of a concentrated hydrochloric acid, stirred at 60° C. for 2 hours, and concentrated under reduced pressure. 80 L of toluene was added to the residue; the mixture was extracted with 150 L of water; and further the water layer was washed with 40 L of toluene. 15.5 L of a 25% NaOH aqueous solution was added to the water layer; the mixture was extracted twice with 80 L and 40 L of toluene; the organic layers were combined and the organic layer was twice washed with 80 L of water; the organic layer was concentrated under reduced pressure; then, 20 L of ethanol was added to the residue; and the mixture was concentrated under reduced pressure to obtain 10.40 kg of a yellow oily target substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08552188B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-4105bc711026474f865574def0062319 |
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| Source note | uspto-grants-2013_10 |
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