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Sodium Hydroxide → [3-Methyl-1-(4-methylpyridin-3-yl)-5-phenyl-1H-pyrazol-4-yl]acetic acid

HRID 888726
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HRID 888726 반응식
[OH-].[Na+].[CH3:3][C:4]1[C:8]([CH2:9][C:10]([O:12]C)=[O:11])=[C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][C:25]=2[CH3:26])[N:5]=1>CO>[CH3:3][C:4]1[C:8]([CH2:9][C:10]([OH:12])=[O:11])=[C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][C:25]=2[CH3:26])[N:5]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 86626934Methyl [3-methyl-1-(4-methylpyridin-3-yl)-5-phenyl-1H-pyrazol-4-yl]acetate

생성물 1

HCID 68818330[3-Methyl-1-(4-methylpyridin-3-yl)-5-phenyl-1H-pyrazol-4-yl]acetic acid

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

0.100 g (2.489 mmol) of 2 molar aqueous sodium hydroxide solution was added to 0.200 g (0.498 mmol) of methyl [3-methyl-1-(4-methylpyridin-3-yl)-5-phenyl-1H-pyrazol-4-yl]acetate in 5.00 ml of methanol, and the mixture was stirred at 20° C. for 1 h. The methanol was removed under reduced pressure, and the residue was poured onto a mixture of 10 ml of water and 15 ml of dichloromethane. The aqueous phase was extracted with 15 ml of dichloromethane, acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. Drying of the combined organic phases and removal of the solvent under reduced pressure give 0.108 g (71% of theory) of a yellow solid of melting point 246° C.

후처리

  1. customThe methanol was removed under reduced pressure
  2. additionthe residue was poured onto a mixture of 10 ml of water and 15 ml of dichloromethane
  3. extractionThe aqueous phase was extracted with 15 ml of dichloromethane
  4. extractionextracted three times with in each case 15 ml of dichloromethane
  5. customDrying of the combined organic phases and removal of the solvent under reduced pressure
  6. customgive 0.108 g (71% of theory) of a yellow solid of melting point 246° C.

출처 및 근거

ORD 기록
ord-a531c57b56a4410ca1282e9efbb24737
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252723B2

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