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Water → HCID 178524945, 화합물

HRID 2182418
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HRID 2182418 반응식
[CH3:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:5][NH:4][N:3]=1.[Mn]([O-])(=O)(=O)=[O:14].[K+].[OH2:19]>C(O)(C)(C)C>[C:7]1([C:6]2[C:2]([C:1]([OH:14])=[O:19])=[N:3][NH:4][CH:5]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
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참가 물질

5

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HCID 962WaterHCID 516875Potassium PermanganateHCID 178434528HCID 178434528, 화합물

생성물 1

HCID 178524945HCID 178524945, 화합물

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A solution of 3-methyl-4-phenylpyrazole (1.00 g) in tert-butanol (15 ml) and water (25 ml), at 60° C., was treated portionwise potassium permanganate (5.47 g). The temperature was then slowly elevated to 90° C. and maintained at that temperature for 5 hours. The mixture was then cooled and filtered through a pad of celite. The filtrate was concentrated and the pH was adjusted to 10 to 14 by addition of 5N aqueous sodium hydroxide solution. This mixture was washed twice with ethyl acetate. The aqueous layer was then acidified to pH 3 to 5 and then extracted four times with ethyl acetate. The combined extracts were dried over magnesium sulfate and then evaporated to yield 4-phenyl-1H-pyrazole-3-carboxylic acid (0.512 g) as a white solid, which was used without further purification. MS:189 (M+H)+. HPLC (METHOD B): RT=2.48 minutes.

후처리

  1. customwas then slowly elevated to 90° C.
  2. temperaturemaintained at that temperature for 5 hours
  3. temperatureThe mixture was then cooled
  4. filtrationfiltered through a pad of celite
  5. concentrationThe filtrate was concentrated
  6. additionthe pH was adjusted to 10 to 14 by addition of 5N aqueous sodium hydroxide solution
  7. washThis mixture was washed twice with ethyl acetate
  8. extractionextracted four times with ethyl acetate
  9. dry with materialThe combined extracts were dried over magnesium sulfate
  10. customevaporated

출처 및 근거

ORD 기록
ord-a693c6f65667437a9c6957c1782fef5c
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06897208B2

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