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Potassium → 4-Phenyl-2-(pyridin-2-yl)-1,2-dihydro-3H-pyrazol-3-one

HRID 977936
ノート
印刷プレビュー

反応式

HRID 977936 の反応式
[K].O[CH:3]=[C:4]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:5]([O:7]CC)=O.Cl.Cl.[NH:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=1)[NH2:19]>C(O)C>[N:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[N:18]1[C:5](=[O:7])[C:4]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[CH:3][NH:19]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5462222PotassiumHCID 64543982-Pyridone hydrazone dihydrochlorideHCID 70430766Ethyl 3-hydroxy-2-phenylprop-2-enoate

生成物 1

HCID 135904734-Phenyl-2-(pyridin-2-yl)-1,2-dihydro-3H-pyrazol-3-one収率 72.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

22.7 g (0.1 mol) of the potassium salt of ethyl α-hydroxymethylene-phenylacetate and 18.2 g (0.1 mol) of 2-hydrazino-pyridine dihydrochloride in 200 ml of ethanol are stirred for 30 minutes at room temperature and then boiled under reflux for 5 hours. After the mixture has been cooled to room temperature, 19.1 g (1.7 mol) of potassium tert.-butylate are introduced in portions while nitrogen is simultaneously passed over the mixture. The mixture is stirred for 4 hours at room temperature and left to stand overnight. The precipitate formed is filtered off under suction and suspended in 100 ml of water, and the suspension is slightly acidified with acetic acid. The crystals are filtered off under suction, washed with water and dried in the air. 17.2 g (72.5% of theory) of 1 -pyrid-2-yl-4-phenyl-pyrazoline-5-one of melting point 132° to 133° C. (ethanol) are obtained.

後処理

  1. temperatureunder reflux for 5 hours
  2. waitleft
  3. waitto stand overnight
  4. customThe precipitate formed
  5. filtrationis filtered off under suction
  6. filtrationThe crystals are filtered off under suction
  7. washwashed with water
  8. customdried in the air

出典と根拠

ORDレコード
ord-02aaffb254624a2ebe1f884cefe0cdc3
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04663327

反応ノート

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