Ethanol → 3-(1-Methylhydrazino)-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine

HRID 27896

反応式

HRID 27896 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([N:8]2[C:12]([CH3:13])=[CH:11][C:10]([CH3:14])=[N:9]2)=[CH:6][CH:7]=1.C(O)C.[CH3:18][NH:19][NH2:20]>O>[CH3:18][N:19]([C:2]1[N:3]=[N:4][C:5]([N:8]2[C:12]([CH3:13])=[CH:11][C:10]([CH3:14])=[N:9]2)=[CH:6][CH:7]=1)[NH2:20]

参加物

5

反応物 3

HCID 702EthanolHCID 6061MethylhydrazineHCID 3210733-Chloro-6-(3,5-dimethylpyrazol-1-yl)pyridazine

生成物 1

HCID 125628643-(1-Methylhydrazino)-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4.17 g (0.02 moles) of 3-chloro-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine, 42 ml of ethanol and 2.3 g (0.05 moles) of methyl hydrazine is heated to reflux for 9 hours, and after cooling the mixture is poured into 100 ml of water. The solution is extracted with 3×50 ml of chloroform and the combined organic phases are dried over magnesium sulphate. After evaporation the residue is recrystallized from a 3:1 mixture of isopropanol and petroleum ether. Yield: 1.9 g (44.5%); m.p.: 93°-94° C.

後処理

  1. temperatureis heated
  2. temperatureto reflux for 9 hours
  3. temperatureafter cooling the mixture
  4. extractionThe solution is extracted with 3×50 ml of chloroform
  5. dry with materialthe combined organic phases are dried over magnesium sulphate
  6. customAfter evaporation the residue
  7. customis recrystallized from a 3:1 mixture of isopropanol and petroleum ether

出典と根拠

ORDレコード
ord-8f3ad70dcc0149729543ac45493e93d6
出典データセット
uspto-grants-1980_09
特許番号
US04224325

関連ノート

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