Pyridinium, 1-methyl-, chloride (1:1) → HCID 20384780、化合物

HRID 26639ノート

反応式

HRID 26639 の反応式
[Cl-].[CH3:2][N+:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>C(OCC)C>[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:6]2[CH:5]=[CH:4][N:3]([CH3:2])[CH2:8][CH:7]=2)[CH2:5][CH2:4]1

参加物

3

反応物 1

HCID 82116Pyridinium, 1-methyl-, chloride (1:1)

生成物 1

HCID 20384780HCID 20384780、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

N,N'-dimethyltetrahydro-4,4'-bipyridyl (DMTB) was prepared from N-methylpyridinium chloride by electrolytic dimerization and obtained in the form of a diethyl ether solution thereof. The so obtained diethyl ether solution was vacuum-distilled to obtain pure DMTB. As the pure DMTB tends to decompose immediately upon contact with oxygen in air, it was carefully handled in a nitrogen atmosphere. A 500 ml three-necked flask was sufficiently washed and dried and then completely filled with nitrogen gas. Into this flask were charged 200 ml of degassed water and 40 millimoles of nitrobenzene. 8 millimoles of DMTB was added, while stirring by rotating a magnetic stirrer having a length of 4 cm at 500 r.p.m., to the mixture charged in the flask, and the reaction was allowed to proceed at room temperature and atmospheric pressure in an atmosphere of nitrogen gas. The measurement of change, with the lapse of time, of pH showed that the pH changed from 6.8 to 12.7 one hour after the initiation of the reaction and it changed no more thereafter.

後処理

  1. distillationwas vacuum-distilled

出典と根拠

ORDレコード
ord-172c0f0cbaff4970b332ef30e5a7fd3b
出典データセット
uspto-grants-1979_04
特許番号
US04151165

反応ノート

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