Methylamine → N-Methyl-2,6-dinitroaniline

HRID 2235530

反応式

HRID 2235530 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 80010N-Methyl-2,6-dinitroaniline収率 91%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b3575c850ed24abfb186b9218c0bcd5c
出典データセット
uspto-grants-2010_05
特許番号
US07714009B2

関連ノート

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