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

HRID 127321

반응식

HRID 127321 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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°.

후처리

  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)

출처 및 근거

ORD 기록
ord-17a4d88615b048d4abf5d8d094c5253d
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255440

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