Potassium Hydroxide → HCID 118436743, compound

HRID 624657Notes

Reaction equation

HRID 624657 reaction equation
[F:1][C:2]([F:15])([F:14])[C:3]([NH:6][CH:7]=[C:8]([CH2:11][C:12]#[N:13])[C:9]#[N:10])([CH3:5])[CH3:4].[OH-].[K+]>CCO.O>[NH2:13][C:12]1[N:6]([C:3]([CH3:5])([CH3:4])[C:2]([F:14])([F:15])[F:1])[CH:7]=[C:8]([C:9]#[N:10])[CH:11]=1

Participants

5

Reactant 2

HCID 14797Potassium HydroxideHCID 900230042-(((1,1,1-Trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile

Product 1

HCID 118436743HCID 118436743, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A solution of 2-(((1,1,1-trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile (187.2 mg, 0.862 mmol) in EtOH (539 μl) was added to a solution of KOH (87 mg, 1.551 mmol) in water (539 μl) at RT. After being stirred at RT for 4 h, the reaction mixture was concentrated under reduced pressure. The residual brown solid was taken up in water and sonicated. The resulting precipitate was collected by filtration, dissolved in EtOAc, washed with brine, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford the title compound as a brown solid, which was used without further purification.

Workup

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customsonicated
  3. filtrationThe resulting precipitate was collected by filtration
  4. dissolutiondissolved in EtOAc
  5. washwashed with brine
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-eff3dbb058754ee5bdfe7dc1b20e21b0
Source dataset
uspto-grants-2016_04
Patent number
US09303045B2

Reaction notes

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