Trifluoroacetic acid → HCID 86718557, compound

HRID 1485035Notes

Reaction equation

HRID 1485035 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[C:16]3[N:17]([C:30]([CH3:33])=[N:31][N:32]=3)[N:18]=[C:19]([N:21]([CH2:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH3:22])[CH:20]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:23]([N:21]([CH3:22])[C:19]1[CH:20]=[C:15]([NH:14][CH:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)[C:16]2[N:17]([C:30]([CH3:33])=[N:31][N:32]=2)[N:18]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 86718558HCID 86718558, compound

Product 1

HCID 86718557HCID 86718557, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

4-[6-(Benzyl-methyl-amino)-3-methyl-[1,2,4]triazolo[4,3-b]pyridazin-8-ylamino]-piperidine-1-carboxylic acid tert-butyl ester (4.08 g; 9.04 mmol) was dissolved in 20.0 ml of DCM and treated with 5.0 ml TFA. It was stirred at ambient temperature for 1 hour. The solution was concentrated under reduced pressure and the residue taken up in DCM and washed with half concentrated NaHCO3 solution. The organic phase was dried over MgSO4 and concentrated.

Workup

  1. concentrationThe solution was concentrated under reduced pressure
  2. washwashed with half concentrated NaHCO3 solution
  3. dry with materialThe organic phase was dried over MgSO4
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-173934ddcf77403f931128862c9609ec
Source dataset
uspto-grants-2016_08
Patent number
US09422290B2

Reaction notes

Loading…