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

HRID 127321ノート

反応式

HRID 127321 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 liters). The solution was heated to boiling and 0.7 liters of solvent were distilled off. The cooled solution was washed with 2N 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 2N 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-17a4d88615b048d4abf5d8d094c5253d
出典データセット
uspto-grants-1981_03
特許番号
US04255440

反応ノート

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