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Sodium Hydroxide → 5-Trifluoromethyl-1-[(3-fluorophenyl)methyl]-1H-pyrrolo[2,3-b]pyridine-2-carboxylic acid

HRID 1690050
ノート
印刷プレビュー

反応式

HRID 1690050 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]2[CH:11]=[CH:10][N:9]([CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)[C:6]2=[N:7][CH:8]=1.CC[C:24]([O-:26])=[O:25].[OH-].[Na+]>C(O)C>[F:21][C:2]([F:20])([F:1])[C:3]1[CH:4]=[C:5]2[CH:11]=[C:10]([C:24]([OH:26])=[O:25])[N:9]([CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)[C:6]2=[N:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 866390575-trifluoromethyl-1-[(3-fluorophenyl)methyl]-1H-pyrrolo[2,3-b]pyridine 2-ethyl carboxylate

生成物 1

HCID 668635175-Trifluoromethyl-1-[(3-fluorophenyl)methyl]-1H-pyrrolo[2,3-b]pyridine-2-carboxylic acid収率 99.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 3.15 g (8.6 mmol) of 5-trifluoromethyl-1-[(3-fluorophenyl)methyl]-1H-pyrrolo[2,3-b]pyridine-2-ethyl carboxylate obtained in Stage 1.2 in 100 mL of ethanol and of 26 mL of 2N sodium hydroxide is stirred for four hours under reflux. After this time, the reaction mixture is concentrated at reduced pressure, and then is taken up in 40 mL of water. The reaction mixture is acidified to pH 3 by successive additions of 1N hydrochloric acid. The precipitate is collected by filtration, washed with water and then dried at reduced pressure. Thus, 2.9 g of the expected product is isolated in the form of a white powder, which is used as it is in the next stage.

後処理

  1. temperatureunder reflux
  2. concentrationAfter this time, the reaction mixture is concentrated at reduced pressure
  3. filtrationThe precipitate is collected by filtration
  4. washwashed with water
  5. customdried at reduced pressure

出典と根拠

ORDレコード
ord-2c190661661e463baf8892acef21b547
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153650B2

反応ノート

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