Sodium Hydroxide → 2-(1-tert-butyl-5-(4-fluorophenyl)-1H-pyrazol-4-yl)thiazole-4-carboxylic acid

HRID 1750364ノート

反応式

HRID 1750364 の反応式
[C:1]([N:5]1[C:9]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[C:8]([C:17]2[S:18][CH:19]=[C:20]([C:22]([O:24]CC)=[O:23])[N:21]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>C(O)C.C1COCC1>[C:1]([N:5]1[C:9]([C:10]2[CH:11]=[CH:12][C:13]([F:16])=[CH:14][CH:15]=2)=[C:8]([C:17]2[S:18][CH:19]=[C:20]([C:22]([OH:24])=[O:23])[N:21]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 86721201ethyl 2-(1-tert-butyl-5-(4-fluorophenyl)-1H-pyrazol-4-yl)thiazole-4-carboxylate

生成物 1

HCID 867212022-(1-tert-butyl-5-(4-fluorophenyl)-1H-pyrazol-4-yl)thiazole-4-carboxylic acid収率 95%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixed solution of the compound (0.57 g, 1.53 mmol) obtained in step 1 and 1N aqueous sodium hydroxide solution (2.289 ml, 2.29 mmol) in ethanol (5 mL) and THF (5 mL) was stirred at 60° C. for 3 hr. The reaction mixture was concentrated under reduced pressure, and 1N hydrochloric acid was added to the residue. The precipitate was collected by filtration to give 2-(1-tert-butyl-5-(4-fluorophenyl)-1H-pyrazol-4-yl)thiazole-4-carboxylic acid (0.50 g, 1.448 mmol, 95%) as a white powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and 1N hydrochloric acid
  2. additionwas added to the residue
  3. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-851add3eefea4350bda1300b9546acf5
出典データセット
uspto-grants-2015_10
特許番号
US09156837B2

反応ノート

読み込み中…