Sodium Hydroxide → 6-(4-Tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid

HRID 2272954ノート

反応式

HRID 2272954 の反応式
C([O:3][C:4]([C:6]1[CH:25]=[C:9]2[C:10](=[O:24])[NH:11][C:12]([C:14]3[CH:19]=[CH:18][C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:16][CH:15]=3)=[CH:13][N:8]2[N:7]=1)=[O:5])C.[OH-].[Na+]>COCCOC>[C:20]([C:17]1[CH:16]=[CH:15][C:14]([C:12]2[NH:11][C:10](=[O:24])[C:9]3[N:8]([N:7]=[C:6]([C:4]([OH:5])=[O:3])[CH:25]=3)[CH:13]=2)=[CH:19][CH:18]=1)([CH3:23])([CH3:21])[CH3:22]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 898263626-(4-Tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid ethyl ester

生成物 1

HCID 898260756-(4-Tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
100 °C

実験手順

A solution of 547 mg (1.61 mmol) 6-(4-tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid ethyl ester in 10 ml 1,2-dimethoxyethane is treated with 5 ml 1 N aqueous NaOH solution. The resulting suspension is heated to 100° C. and the resulting solution is stirred at this temperature for 48 hours. The reaction mixture is cooled to room temperature and evaporated. The residue is triturated with water and the solids are filtered off and washed with water. The filtrate is acidified with 2 N HCl. The resulting precipitate is filtered off, washed with 2 N HCl and with water and dried under vacuum to give 6-(4-tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid as colourless solid; HPLC/MS 2.03 (A), [M+H] 312.

後処理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. customevaporated
  3. customThe residue is triturated with water
  4. filtrationthe solids are filtered off
  5. washwashed with water
  6. filtrationThe resulting precipitate is filtered off
  7. washwashed with 2 N HCl and with water
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-a465ef600bf84b749356f93286087419
出典データセット
uspto-grants-2015_09
特許番号
US09120805B2

反応ノート

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