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Methylhydrazine → HCID 21441230, 화합물

HRID 1658350
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HRID 1658350 반응식
[CH3:1][NH:2][NH2:3].[C:4]1([C:10](=O)[CH:11]([CH2:20][CH3:21])[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=O)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>C(O)(C)C>[C:4]1([C:10]2[C:11]([CH2:20][CH3:21])=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:2]([CH3:1])[N:3]=2)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 105149681,3-Propanedione, 2-ethyl-1,3-diphenyl-

생성물 1

HCID 21441230HCID 21441230, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
80 °C

실험 절차

Methylhydrazine (2.86 g, 0.06 mole) is added to an isopropanol (100 ml) solution of 1,3-diphenyl-2-ethyl-1,3-propanedione (11.0 g, 0.044 mole) with constant stirring at 80°C. The reaction mixture is heated at reflux for 31/2 hours, then stirred at room temperature overnight. The reaction mixture is poured into ice water, stirred for 1/2 hour, and the resulting mixture extracted with chloroform (3×50 ml). Evaporation of the organic layer gives an oil which is crystallized from hexane with cooling to give 6.47 g (56%) or product, m.p. 80° to 81°C.

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for 31/2 hours
  3. stirringstirred at room temperature overnight
  4. stirringstirred for 1/2 hour
  5. extractionthe resulting mixture extracted with chloroform (3×50 ml)
  6. customEvaporation of the organic layer
  7. customgives an oil which
  8. customis crystallized from hexane
  9. temperaturewith cooling
  10. customto give 6.47 g (56%) or product, m.p. 80° to 81°C.

출처 및 근거

ORD 기록
ord-b69c33edcdc84007a4a33b540a44a434
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03963741

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