Methylamine → N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine

HRID 426488

反応式

HRID 426488 の反応式
[CH3:1][NH2:2].C(O)C.C(Cl)CCl.[CH3:10][S:11][C:12](SC)=[CH:13][N+:14]([O-:16])=[O:15]>C(Cl)CCl>[CH3:1][NH:2][CH:12]([S:11][CH3:10])[CH2:13][N+:14]([O-:16])=[O:15]

参加物

5

反応物 3

HCID 6329MethylamineHCID 836231,1-Bis(methylthio)-2-nitroethyleneHCID 229016121,2-Dichloroethane ethanol

生成物 1

HCID 15788612N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A solution of methylamine in ethanol/ethylenedichloride (112.5 ml of 33% ethanolic methylamine in 0.8 liters of ethylene dichloride; 0.94 mole) was added over 51/2 hr at 70° to a stirred solution of 1,1-bismethylthio-2-nitroethene (99.0 g, 0.6 mole) in ethylene dichloride (1.5 litres). The solution was heated to boiling and 0.7 liters of solvent were distilled off. The cooled solution was washed with 2 N hydrochloric acid (0.25 liters), then with brine (0.25 liters). The solvent was removed and the residue crystallised from isopropyl acetate (0.5 liters), treating the hot solution with charcoal (10.0 g). The product (35.0 g) formed yellow prisms, m.p. 114°.

後処理

  1. temperatureThe solution was heated
  2. distillation0.7 liters of solvent were distilled off
  3. washThe cooled solution was washed with 2 N hydrochloric acid (0.25 liters)
  4. customThe solvent was removed
  5. customthe residue crystallised from isopropyl acetate (0.5 liters)
  6. additiontreating the hot solution with charcoal (10.0 g)

出典と根拠

ORDレコード
ord-398c82f5d14c448492bab9c8b502c38c
出典データセット
uspto-grants-1979_10
特許番号
US04169855

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