Sodium Hydroxide → 2-(6-methylpyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole-3-carboxylic acid

HRID 8233ノート

反応式

HRID 8233 の反応式
C([O:3][C:4]([C:6]1[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[N:12]=2)=[N:9][N:8]2[CH2:18][CH2:19][CH2:20][C:7]=12)=[O:5])C.[OH-].[Na+]>C(O)C>[CH3:17][C:13]1[N:12]=[C:11]([C:10]2[C:6]([C:4]([OH:5])=[O:3])=[C:7]3[CH2:20][CH2:19][CH2:18][N:8]3[N:9]=2)[CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 693657412-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole-3-carboxylic acid ethyl ester

生成物 1

HCID 219925742-(6-methylpyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole-3-carboxylic acid ethyl ester (1.6 g, 5.9 mmol) and 2 N sodium hydroxide (6 mL, 29 mmol) in absolute ethanol (50 mL) is refluxed for 5 h. The mixture is cooled to room temperature and concentrated in vacuo. The residue is suspended in water and acidified to pH 5 with 1 N hydrochloric acid. The aqueous solution is extracted three times with dichloromethane. The organic extracts are combined, dried (sodium sulfate), filtered, and concentrated in vacuo to yield the title compound, 1.4 g (97%), as a white solid.

後処理

  1. concentrationconcentrated in vacuo
  2. extractionThe aqueous solution is extracted three times with dichloromethane
  3. dry with materialdried (sodium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-096d773aff6c4128951312bff972383e
出典データセット
uspto-grants-2006_08
特許番号
US07087626B2

反応ノート

読み込み中…