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

HRID 2170875ノート

反応式

HRID 2170875 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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 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

後処理

  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

出典と根拠

ORDレコード
ord-107ce1c7eef74e15b1a2221eac4e0019
出典データセット
uspto-grants-2015_06
特許番号
US09051304B2

反応ノート

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