Sodium Hydroxide → HCID 178469580、化合物

HRID 497948

反応式

HRID 497948 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([NH:7][CH:8]=[C:9]([C:15]([O:17]CC)=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[N:4]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[N:3]=1.[OH-].[Na+]>O>[OH:17][C:15]1[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:8][N:7]=[C:5]2[N:4]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[N:3]=[C:2]([CH3:1])[C:6]=12

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22320362Diethyl 2-([[3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]methylene)malonate

生成物 1

HCID 178469580HCID 178469580、化合物収率 57%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A solution of diethyl 2-([[3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]methylene)malonate (2.0 g, 5.8 mmol) in polyphosphoric acid (10 g) was heated and stirred at 100° C. for 2 hours. The solution was cooled to room temperature, and iced water was added thereto. The solution was neutralized by the addition of an aqueous sodium hydroxide solution, and organic matter was extracted with 10% methanol/chloroform. The extract was washed with saturated brine and water, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Purification of the residue by silica gel column chromatography (chloroform) gave the title compound (0.98 g, 57% yield).

後処理

  1. temperatureThe solution was cooled to room temperature
  2. extractionwas extracted with 10% methanol/chloroform
  3. washThe extract was washed with saturated brine and water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customPurification of the residue by silica gel column chromatography (chloroform)

出典と根拠

ORDレコード
ord-ef246cbc7ab649d8bdb7ede3513c10f7
出典データセット
uspto-grants-2005_09
特許番号
US06949648B2

関連ノート

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