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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
ノート
印刷プレビュー

反応式

HRID 352821 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 30856Mercuric oxide触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2854f45b84e748d596a35ef1814faa13
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06747023B1

反応ノート

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