1,2-Dimethylhydrazine → 3-(2-Aminoethylamino)-1,2,4-trimethylpyrazol-5-one

HRID 2164906노트

반응식

HRID 2164906 반응식
Cl[C:2]1[N:3]([CH3:10])[N:4]([CH3:9])[C:5](=[O:8])[C:6]=1[CH3:7].OC1N(C)[N:14](C)[C:15](=O)[C:16]=1C.CC(C(OCC)=O)C(OCC)=O.C[NH:34]NC.P(Cl)(Cl)(Cl)=O>>[NH2:34][CH2:16][CH2:15][NH:14][C:2]1[N:3]([CH3:10])[N:4]([CH3:9])[C:5](=[O:8])[C:6]=1[CH3:7]

참가 물질

6

반응물 5

HCID 13221,2-DimethylhydrazineHCID 11857Diethyl methylmalonateHCID 24813Phosphorus oxychlorideHCID 128188533-Hydroxy-1,2,4-trimethyl-5-pyrazoloneHCID 128188543-Chloro-1,2,4-trimethylpyrazol-5-one2회

생성물 1

HCID 128188553-(2-Aminoethylamino)-1,2,4-trimethylpyrazol-5-one

실험 절차

The 3-chloro-1,2,4-trimethylpyrazol-5-one used as starting material can be obtained in the following manner: 28.6 g. 3-hydroxy-1,2,4-trimethylpyrazol-5-one (m.p. 87°-89° C., after recrystallization from ethyl acetate), prepared from diethyl methylmalonate and N,N'-dimethylhydrazine, are boiled under reflux for 3.5 hours with 55 ml. phosphorus oxychloride. The reaction mixture is then evaporated and the residue is stirred with ice and water, rendered alkaline by the addition of 10N aqueous sodium hydroxide solution and extracted 8 times with 100 ml. amounts of methylene chloride. The combined extracts are then dried and evaporated to give 24.7 g. (76.5% of theory) 3-chloro-1,2,4-trimethylpyrazol-5-one in the form of colorless crystals; m.p. 37°-38° C.

후처리

  1. customcan be obtained in the following manner
  2. temperatureunder reflux for 3.5 hours with 55 ml
  3. customThe reaction mixture is then evaporated
  4. additionby the addition of 10N aqueous sodium hydroxide solution
  5. extractionextracted 8 times with 100 ml
  6. customThe combined extracts are then dried
  7. customevaporated
  8. customto give 24.7 g

출처 및 근거

ORD 기록
ord-fb3ef9226dad4925a7e1936de36c70f8
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04507488

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