Trifluoroacetic acid → HCID 21098120, compound

HRID 1351081Notes

Reaction equation

HRID 1351081 reaction equation
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][N:18]([C:21]2[N:22]([CH2:45][C:46]#[C:47][CH3:48])[C:23]3[C:28](=[O:29])[N:27]([CH2:30][C:31]4[CH:32]=[C:33]5[C:38](=[C:39]([CH3:41])[CH:40]=4)[N:37]=[C:36]([CH3:42])[C:35]([CH3:43])=[N:34]5)[N:26]=[CH:25][C:24]=3[N:44]=2)[CH2:17][CH2:16]1)=O)(C)(C)C>C(Cl)Cl>[N:18]1([C:21]2[N:22]([CH2:45][C:46]#[C:47][CH3:48])[C:23]3[C:28](=[O:29])[N:27]([CH2:30][C:31]4[CH:32]=[C:33]5[C:38](=[C:39]([CH3:41])[CH:40]=4)[N:37]=[C:36]([CH3:42])[C:35]([CH3:43])=[N:34]5)[N:26]=[CH:25][C:24]=3[N:44]=2)[CH2:19][CH2:20][NH:15][CH2:16][CH2:17]1

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 21098101HCID 21098101, compound

Product 1

HCID 21098120HCID 21098120, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

2 ml of trifluoroacetic acid are added to 220 mg of 2-(4-tert.-butyloxycarbonyl-piperazin-1-yl)-3-(2-butyn-1-yl)-5-[(2,3,8-trimethyl-quinoxalin-6-yl)methyl]-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one in 4 ml methylene chloride. The reaction mixture is stirred for one hour at ambient temperature. Then it is diluted with methylene chloride and washed with saturated sodium hydrogen carbonate solution. The organic phase is dried and evaporated down. The glassy residue is dissolved in dioxane, frozen with liquid nitrogen and dried at 6×10−3 mbar. A white solid remains.

Workup

  1. washwashed with saturated sodium hydrogen carbonate solution
  2. customThe organic phase is dried
  3. customevaporated down
  4. dissolutionThe glassy residue is dissolved in dioxane
  5. temperaturefrozen with liquid nitrogen
  6. customdried at 6×10−3 mbar

Sources & evidence

ORD record
ord-4aa02fa9d49541f3a8072ef7df4d5e0f
Source dataset
uspto-grants-2007_05
Patent number
US07217711B2

Reaction notes

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