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Sodium Hydroxide → [3-Methyl-5-phenyl-1-(pyrazin-2-yl)-1H-pyrazol-4-yl]acetic acid

HRID 2068479
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HRID 2068479 반응식
[OH-].[Na+].C[O:4][C:5](=[O:25])[CH2:6][C:7]1[C:8]([CH3:24])=[N:9][N:10]([C:18]2[CH:23]=[N:22][CH:21]=[CH:20][N:19]=2)[C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CO>[CH3:24][C:8]1[C:7]([CH2:6][C:5]([OH:25])=[O:4])=[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:10]([C:18]2[CH:23]=[N:22][CH:21]=[CH:20][N:19]=2)[N:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 131730041methyl[3-methyl-5-phenyl-1-(pyrazin-2-yl)-1H-pyrazol-4-yl]acetate

생성물 1

HCID 67028937[3-Methyl-5-phenyl-1-(pyrazin-2-yl)-1H-pyrazol-4-yl]acetic acid

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

0.073 g (1.819 mmol) of 2-molar aqueous sodium hydroxide solution was added to 0.165 g (0.455 mmol) of methyl[3-methyl-5-phenyl-1-(pyrazin-2-yl)-1H-pyrazol-4-yl]acetate (see A3) dissolved in 5 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 into 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 gave 0.080 g (59.7% of theory) of a colorless foamy solid, melting point 125° C.

후처리

  1. customThe methanol was removed under reduced pressure
  2. additionthe residue was poured into 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. customgave 0.080 g (59.7% of theory) of a colorless foamy solid, melting point 125° C.

출처 및 근거

ORD 기록
ord-646855cf86da4a5ab47b45b0068ad7c5
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08298994B2

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