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Ethyl 5-hydrazino-3-(pyridin-4-yl)-1,2,4-triazine-6-carboxylate → Ethyl 3-(pyridin-4-yl)-1,2,4-triazin-6-carboxylate

HRID 352821
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HRID 352821 반응식
N([C:3]1[N:4]=[C:5]([C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)[N:6]=[N:7][C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10])N>C(O)C.[Hg]=O>[N:17]1[CH:18]=[CH:19][C:14]([C:5]2[N:6]=[N:7][C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:3][N:4]=2)=[CH:15][CH:16]=1
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참가 물질

4

반응물 1

HCID 22709653Ethyl 5-hydrazino-3-(pyridin-4-yl)-1,2,4-triazine-6-carboxylate

생성물 1

HCID 22711342Ethyl 3-(pyridin-4-yl)-1,2,4-triazin-6-carboxylate수율 52%

시약·촉매·용매 2

HCID 30856Mercuric oxide촉매HCID 702Ethanol용매

실험 절차

In ethanol (5 ml) was suspended ethyl 5-hydrazino-3-(pyridin-4-yl)-1,2,4-triazine-6-carboxylate (50 mg). To the resulting suspension, mercury (II) oxide (98 mg) was added and the resulting mixture was heated under reflux for 9 hours. After completion of the reaction, the insoluble matter was removed through Celite filtration. The filtrate was concentrated and the concentrate was separated into layers by the addition of ethyl acetate and water. The organic layer thus obtained was dried over anhydrous magnesium sulfate. The filtrate was concentrated, whereby a crudely purified product of the title compound (23 mg, pale yellow powder) was obtained.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 9 hours
  3. customAfter completion of the reaction
  4. customthe insoluble matter was removed through Celite filtration
  5. concentrationThe filtrate was concentrated
  6. customthe concentrate was separated into layers by the addition of ethyl acetate and water
  7. customThe organic layer thus obtained
  8. dry with materialwas dried over anhydrous magnesium sulfate
  9. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-2854f45b84e748d596a35ef1814faa13
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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