Methylamine → N-Methyl-2,6-dinitroaniline

HRID 2235530

반응식

HRID 2235530 반응식
[CH3:1][NH2:2].Cl[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:5]=1[N+:13]([O-:15])=[O:14]>C1COCC1>[CH3:1][NH:2][C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:5]=1[N+:13]([O-:15])=[O:14]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 118141-Chloro-2,6-dinitrobenzene

생성물 1

HCID 80010N-Methyl-2,6-dinitroaniline수율 91%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methylamine (4.5 ml of 2.0 M solution in THF) was added to a stirred solution of 2-chloro-1,3-dinitrobenzene (0.90 g, 4.4 mmol) in 40 ml of THF and the mixture was stirred for 30 min. The reaction was quenched by the addition of water and ether. The aqueous layer was separated and extracted twice with ether. The combined organic extracts were washed with saturated NaHCO3, brine and dried over magnesium sulfate. Filtration, removal of solvent and purification of residue via Biotage chromatography eluting with 20% ethyl acetate/dichloromethane to gave 0.80 g (91%) of product.

후처리

  1. customThe reaction was quenched by the addition of water and ether
  2. customThe aqueous layer was separated
  3. extractionextracted twice with ether
  4. washThe combined organic extracts were washed with saturated NaHCO3, brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationFiltration, removal of solvent and purification of residue via Biotage chromatography
  7. washeluting with 20% ethyl acetate/dichloromethane

출처 및 근거

ORD 기록
ord-b3575c850ed24abfb186b9218c0bcd5c
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714009B2

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