1,1-Dimethylhydrazine → HCID 299783, 화합물

HRID 1729604노트

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HRID 1729604 반응식
[N:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:2].[CH3:9][N:10]([NH2:12])[CH3:11]>C(O)C>[CH3:9][N:10]([CH3:11])[N:12]=[N+:1]([O-:2])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 59761,1-DimethylhydrazineHCID 11473Nitrosobenzene

생성물 1

HCID 299783HCID 299783, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
25 °C

실험 절차

To a solution of 7.5 g. of nitrosobenzene in 80 ml. of ethanol at 0° was added in a dropwise manner 4.2 g. of unsymmetrical-dimethylhydrazine as a saturated solution in ethanol. After stirring at 0° for 2 hours, the reaction mixture was allowed to warm to 25° C. and stirred for 16 hours longer. The solution was concentrated in vacuo, and the red-brown oil was chromatographed on silica gel in benzene. The product was eluted with 5-10 percent ethyl acetate in benzene. Three grams of 3,3-dimethyl-1-phenyltriazene-1-oxide was obtained as a light brown oil which gave a suitable n.m.r. spectrum.

후처리

  1. stirringstirred for 16 hours longer
  2. concentrationThe solution was concentrated in vacuo
  3. customthe red-brown oil was chromatographed on silica gel in benzene
  4. washThe product was eluted with 5-10 percent ethyl acetate in benzene

출처 및 근거

ORD 기록
ord-67888d494fa040e192812873e2f4a505
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03989680

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