Potassium Hydroxide → HCID 118436743、化合物

HRID 624657ノート

反応式

HRID 624657 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 118436743HCID 118436743、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-eff3dbb058754ee5bdfe7dc1b20e21b0
出典データセット
uspto-grants-2016_04
特許番号
US09303045B2

反応ノート

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