Hydrochloric Acid → HCID 178478964, compound

HRID 1851252Notes

Reaction equation

HRID 1851252 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[N:18]=[C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[N:20]=3)[NH:16][N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:29]>O1CCOCC1.CCOCC>[ClH:29].[NH:8]1[CH2:9][CH2:10][CH:11]([C:14]2[N:18]=[C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:27])([F:28])[F:26])[N:20]=3)[NH:16][N:15]=2)[CH2:12][CH2:13]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 178451824HCID 178451824, compound

Product 1

HCID 178478964HCID 178478964, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 312751,4-DioxaneSolvent

Procedure

A mixture of 4-[5-(6-trifluoromethyl-pyridine-2-yl)-1H-[1,2,4]triazol-3-yl]-piperidine-1-carboxylic acid tert-butyl ester (3.26 g) and 4M HCl in dioxane (47 mL) was stirred at rt until the reaction was complete. The reaction was diluted with Et2O and stirred for 30 minutes. The solid was filtered, taken up in ACN and stirred for 15 minutes. The solid was filtered, dissolved in warm MeOH, cooled to 0° C. and triturated with Et2O. The resulting solid was filtered and dried to give the title compound.

Workup

  1. stirringstirred for 30 minutes
  2. filtrationThe solid was filtered
  3. stirringstirred for 15 minutes
  4. filtrationThe solid was filtered
  5. dissolutiondissolved in warm MeOH
  6. temperaturecooled to 0° C.
  7. customtriturated with Et2O
  8. filtrationThe resulting solid was filtered
  9. customdried

Sources & evidence

ORD record
ord-24fb283b4a8b456298b8d69277575c22
Source dataset
uspto-grants-2015_02
Patent number
US08957064B2

Reaction notes

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