Dimethylamine → HCID 25183728, compound

HRID 80718Notes

Reaction equation

HRID 80718 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]4)=[N:12][N:11]3[C:23]=2[C:24]2[CH:29]=[CH:28][N:27]=[C:26](F)[CH:25]=2)=[CH:4][CH:3]=1.[CH3:31][NH:32][CH3:33]>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:17][CH2:18][N:19]([CH3:22])[CH2:20][CH2:21]4)=[N:12][N:11]3[C:23]=2[C:24]2[CH:29]=[CH:28][N:27]=[C:26]([N:32]([CH3:33])[CH3:31])[CH:25]=2)=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 674DimethylamineHCID 59406951HCID 59406951, compound

Product 1

HCID 25183728HCID 25183728, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
150 °C

Procedure

0.10 g (0.25 mmol) of 2-(4-fluorophenyl)-3-(2-fluoropyrid-4-yl)-6-(4-methylpiperazin-1-yl)imidazo[1,2-b]pyridazine and 10 mL of dimethylamine are introduced into an autoclave. The mixture is heated at 150° C. overnight and then cooled and poured into water. The product is extracted with chloroform, and the organic phase is dried over sodium sulfate and then concentrated under reduced pressure to give a solid. This solid is crystallized and recrystallized from acetonitrile to give 0.028 g of a white powder after cooling, filtering off and drying.

Workup

  1. temperaturecooled
  2. extractionThe product is extracted with chloroform
  3. dry with materialthe organic phase is dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give a solid
  6. customThis solid is crystallized
  7. customrecrystallized from acetonitrile

Sources & evidence

ORD record
ord-48c50ffd20ec4e52a04c128936ffec1d
Source dataset
uspto-grants-2014_09
Patent number
US08846676B2

Reaction notes

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