1,1-Dimethylhydrazine → HCID 299783、化合物

HRID 1729604ノート

反応式

HRID 1729604 の反応式
[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

参加物

4

反応物 2

HCID 59761,1-DimethylhydrazineHCID 11473Nitrosobenzene

生成物 1

HCID 299783HCID 299783、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-67888d494fa040e192812873e2f4a505
出典データセット
uspto-grants-1976_11
特許番号
US03989680

反応ノート

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