Sodium Hydroxide → 2-(4-Fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinic acid

HRID 1908274노트

반응식

HRID 1908274 반응식
[F:1][C:2]1[C:3]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:4][N:5]([C:7]2[N:17]=[CH:16][CH:15]=[CH:14][C:8]=2[C:9]([O:11]CC)=[O:10])[CH:6]=1.[OH-].[Na+]>CO>[F:1][C:2]1[C:3]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[N:4][N:5]([C:7]2[N:17]=[CH:16][CH:15]=[CH:14][C:8]=2[C:9]([OH:11])=[O:10])[CH:6]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 67238757ethyl 2-(4-fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinate

생성물 1

HCID 672390012-(4-Fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinic acid수율 90.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To ethyl 2-(4-fluoro-3-phenyl-1H-pyrazol-1-yl)nicotinate (1.49 g, 4.79 mmol) in methanol (40 ml) 8.5 ml of an aqueous 2 m NaOH-solution (17 mmol) was added dropwise at 10° C., and the mixture was stirred for 2 h at room temperature and then for 3 h at 65° C. After completion of the reaction the mixture was concentrated under reduced pressure, dissolved in water and acidified using 2 n HCl. The precipitate formed was filtered off, washed with water and dried to give 1.23 g of a white amorphous solid; ESI-MS [M+H]+: 284.1.

후처리

  1. waitfor 3 h at 65° C
  2. customAfter completion of the reaction the mixture
  3. concentrationwas concentrated under reduced pressure
  4. dissolutiondissolved in water
  5. customThe precipitate formed
  6. filtrationwas filtered off
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-2c44cc29812d48248647ce317ed06064
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598211B2

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