Chloroform → 3,5-Dimethylpyrazole-1-carboxamidine

HRID 2395220ノート

反応式

HRID 2395220 の反応式
[OH-].[K+].C(Cl)(Cl)Cl.Cl.[C:8]([N:11]1[C:15]([CH3:16])=[CH:14][C:13]([CH3:17])=[N:12]1)(=[NH:10])[NH2:9]>O>[C:8]([N:11]1[C:15]([CH3:16])=[CH:14][C:13]([CH3:17])=[N:12]1)(=[NH:9])[NH2:10]

参加物

5

反応物 3

HCID 6212ChloroformHCID 14797Potassium HydroxideHCID 2180023,5-Dimethylpyrazole-1-carboxamidine monohydrochloride

生成物 1

HCID 975253,5-Dimethylpyrazole-1-carboxamidine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To 850 ml of ethanol were added 188 g of aminoguanidine hydrochloride and 170 g of 2,4-pentadione and the mixture was heated with stirring for 3 hrs. under reflux. The precipitated crystals were filtered, sufficiently washed with ethanol and dried to obtain 1-amidino-3,5-dimethylpyrazole hydrochloride of 210 g. Next, 60 g of potassium hydroxide was dissolved in water of 120 g and 1-amidino-3,5-dimethylpyrazole hydrochloride of 61.1 g was added thereto withcooling with water and stirred further for 1 hr. Chloroform of 200 ml was added to the solution for extraction. A chloroform layer was separated, washed with water and dried with anhydrous sodium sulfate, thereafter, chloroform was removed to obtain 1-amidino-3,5-dimethylpyrazole of 46.0 g.

後処理

  1. additionwas added
  2. customA chloroform layer was separated
  3. washwashed with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. customchloroform was removed

出典と根拠

ORDレコード
ord-b96d879cf8e347c1978c106333837840
出典データセット
uspto-grants-1998_09
特許番号
US05814580

反応ノート

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