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

HRID 2272954노트

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HRID 2272954 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a465ef600bf84b749356f93286087419
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09120805B2

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