Trifluoroacetic acid → HCID 68501107, compound

HRID 2381076Notes

Reaction equation

HRID 2381076 reaction equation
C(O)(C(F)(F)F)=O.[F:8][C:9]([F:33])([F:32])[C:10]1[N:14]2[N:15]=[C:16]([N:19]3[CH2:24][CH2:23][N:22](C(OC(C)(C)C)=O)[CH2:21][CH2:20]3)[CH2:17][CH2:18][C:13]2=[N:12][N:11]=1>C(Cl)Cl>[N:19]1([C:16]2[CH2:17][CH2:18][C:13]3[N:14]([C:10]([C:9]([F:8])([F:32])[F:33])=[N:11][N:12]=3)[N:15]=2)[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]1

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 68499878HCID 68499878, compound

Product 1

HCID 68501107HCID 68501107, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

TFA (5 mL) was added to tert-butyl 4-[3-(trifluoromethyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperazine-1-carboxylate (1.88 g, 5.02 mmol) in DCM (5 mL). The resulting solution was stirred at ambient temperature for 30 minutes then added to a SCX column. The desired product was eluted from the column using 2M ammonia in methanol and the solvents were evaporated to dryness to give 6-(piperazin-1-yl)-3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazine (1.360 g, 99%) as a solid.

Workup

  1. additionthen added to a SCX column
  2. washThe desired product was eluted from the column
  3. customthe solvents were evaporated to dryness

Sources & evidence

ORD record
ord-502a263a511b4dcdbbefa94f9039f230
Source dataset
uspto-grants-2012_09
Patent number
US08258140B2

Reaction notes

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