Chloroform → 3,5-Dimethylpyrazole-1-carboxamidine

HRID 2395220노트

반응식

HRID 2395220 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 975253,5-Dimethylpyrazole-1-carboxamidine

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b96d879cf8e347c1978c106333837840
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05814580

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