Hydrochloric Acid → HCID 18723226, compound

Temperature

60 °C

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.

1. stirringstirred at 60° C. for 2 hours
2. concentrationconcentrated under reduced pressure
3. addition80 L of toluene was added to the residue
4. extractionthe mixture was extracted with 150 L of water
5. washand further the water layer was washed with 40 L of toluene
6. addition15.5 L of a 25% NaOH aqueous solution was added to the water layer
7. extractionthe mixture was extracted twice with 80 L and 40 L of toluene
8. washthe organic layer was twice washed with 80 L of water
9. concentrationthe organic layer was concentrated under reduced pressure
10. additionthen, 20 L of ethanol was added to the residue
11. concentrationand the mixture was concentrated under reduced pressure
12. customto obtain 10.40 kg of a yellow oily target substance

ORD record

ord-4046a1d16d054edb8d3450f688ca20bc

Source dataset

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08344148B2