Sodium Hydroxide → HCID 178469580, 화합물

HRID 497948

반응식

HRID 497948 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178469580HCID 178469580, 화합물수율 57%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-ef246cbc7ab649d8bdb7ede3513c10f7
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949648B2

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