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Hydrochloric Acid → 2-(4-Methylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 889303
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반응식

HRID 889303 반응식
C(O[C:4](=[O:14])[C:5]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=[CH:6]O)C.[NH:15]([C:17]1[CH:22]=[C:21]([CH3:23])[CH:20]=[CH:19][N:18]=1)[NH2:16].C([O-])C.[Na+].Cl>C(O)C>[CH3:23][C:21]1[CH:20]=[CH:19][N:18]=[C:17]([N:15]2[C:4](=[O:14])[C:5]([C:8]3[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=3)=[CH:6][NH:16]2)[CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 122667392-Hydrazinyl-4-methylpyridineHCID 687080883-Hydroxy-2-pyridin-3-yl-acrylic acid ethyl ester

생성물 1

HCID 591869542-(4-Methylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

1.53 g (7.90 mmol) of the compound from Example 2A and 2.92 g (23.7 mmol) of the compound from Example 1A are dissolved 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 16 h. 537 g (7.90 mmol) sodium ethanolate are added, the reaction solution becoming dark red in color. The mixture is subsequently stirred at RT for 30 min and 7.9 ml 1 M hydrochloric acid are then added. The solution is partly concentrated, a precipitate separating out. This is filtered off, washed with water (twice with 5 ml each time) and with MTBE (5 ml) and dried in vacuo. 435 mg (22% of th.) of the title compound are obtained.

후처리

  1. stirringThe mixture is subsequently stirred at RT for 30 min
  2. concentrationThe solution is partly concentrated
  3. customa precipitate separating out
  4. filtrationThis is filtered off
  5. washwashed with water (twice with 5 ml each time) and with MTBE (5 ml)
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-63bf55f4b9034805bcbdb450d41003c6
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252817B2

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