HCID 68959286, compound → HCID 136387223, compound

HRID 1396559Notes

Reaction equation

HRID 1396559 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([C:11]2[C:19]3[C:14](=[N:15][C:16]([NH2:20])=[N:17][CH:18]=3)[N:13]([CH3:21])[N:12]=2)[CH:5]=[C:6]([F:10])[C:7]=1[O:8]C>Br.O>[NH2:20][C:16]1[N:15]=[C:14]2[N:13]([CH3:21])[N:12]=[C:11]([C:4]3[CH:5]=[C:6]([F:10])[C:7]([OH:8])=[C:2]([F:1])[CH:3]=3)[C:19]2=[CH:18][N:17]=1

Participants

4

Reactant 1

HCID 68959286HCID 68959286, compound

Product 1

HCID 136387223HCID 136387223, compound

Reagents, catalysts & solvents 2

HCID 260Hydrogen BromideSolventHCID 962WaterSolvent

Procedure

3-(3,5-Difluoro-4-methoxy-phenyl)-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-6-ylamine (Example 98) (0.1 g, 0.342 mmol) is dissolved in 48% HBr in water (5 ml) and heated using microwave radiation at 120° C. for 30 minutes. Purification of the reaction mixture by preparative HPLC (water/acetonitrile, 0.1% TFA) affords the title compound as a white solid.

Workup

  1. temperatureheated
  2. customat 120° C.
  3. customfor 30 minutes
  4. customPurification of the reaction mixture by preparative HPLC (water/acetonitrile, 0.1% TFA)

Sources & evidence

ORD record
ord-85b6bc10c55c4f2193451f02d3026751
Source dataset
uspto-grants-2014_12
Patent number
US08901134B2

Reaction notes

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