Dimethylamine → HCID 25183728, compound

HRID 1803884Notes

Reaction equation

HRID 1803884 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-e97b86c27e384d4d90f03eb06b226c86
Source dataset
uspto-grants-2013_01
Patent number
US08354405B2

Reaction notes

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