Hydrochloric Acid → 4-Pyridin-3-yl-2-pyrimidin-2-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 889302

반응식

HRID 889302 반응식
C(O[C:4](=[O:14])[C:5]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=[CH:6]O)C.[NH:15]([C:17]1[N:22]=[CH:21][CH:20]=[CH:19][N:18]=1)[NH2:16].[H-].[Na+].Cl>C(O)C>[N:10]1[CH:11]=[CH:12][CH:13]=[C:8]([C:5]2[C:4](=[O:14])[N:15]([C:17]3[N:22]=[CH:21][CH:20]=[CH:19][N:18]=3)[NH:16][CH:6]=2)[CH:9]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 3465582-HydrazinylpyrimidineHCID 687080883-Hydroxy-2-pyridin-3-yl-acrylic acid ethyl ester

생성물 1

HCID 591869714-Pyridin-3-yl-2-pyrimidin-2-yl-1,2-dihydro-3H-pyrazol-3-one

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

193 mg (1 mmol) of the compound from Example 2A and 116 mg (1.05 mmol) 2-hydrazinopyrimidine are initially introduced into 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 20 h. 40 mg (1 mmol) sodium hydride suspension (60% strength in paraffin oil) are then added in portions, a significant clouding of the reaction solution developing. The mixture is subsequently stirred at RT for 10 min. 1 ml 1 M hydrochloric acid is then added to the dark reaction mixture, a precipitate separating out. The precipitate is filtered off with suction and the residue is washed with water (2×1 ml) and dried in vacuo. 173 mg (72% of th.) of the title compound are obtained.

후처리

  1. stirringThe mixture is subsequently stirred at RT for 10 min
  2. customa precipitate separating out
  3. filtrationThe precipitate is filtered off with suction
  4. washthe residue is washed with water (2×1 ml)
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-070ffdff072d47598df30111070eeaa4
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252817B2

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