Dimethyl Sulfoxide → 2-(Methylamino)-6-methyl-3,5-dinitropyridine

HRID 1974016ノート

反応式

HRID 1974016 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[C:4]([CH3:14])[N:3]=1.[CH3:15]S(C)=O.CN>CN(C)C(=O)C.O>[CH3:15][NH:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[C:4]([CH3:14])[N:3]=1

参加物

6

反応物 3

HCID 679Dimethyl SulfoxideHCID 6329MethylamineHCID 2853032-Amino-3,5-dinitro-6-methylpyridine

生成物 1

HCID 135670252-(Methylamino)-6-methyl-3,5-dinitropyridine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of 2-amino-6-methyl-3,5-dinitropyridine (24.9 g, 0.125 mole) and 175 ml dimethylsulfoxide in a 500 ml Parr bottle was added a solution of methylamine (20 g, 0.65 mole) in 75 ml N,N-dimethylacetamide. The reaction was shaken for 6 hours at ambient temperature and then heated 15 hours at 70° C. Upon cooling, the mixture was diluted with water, filtered, washed with methanol-water (1v/1v) and dried. 2-(methylamino)-6-methyl-3,5-dinitropyridine was obtained as a yellow solid (82% yield). Anal. Calcd. for C7H8N4O4 : C, 39.6; H, 3.8; N, 26.4. Found: C, 39.6; H, 3.9; N, 26.3.

後処理

  1. temperatureheated 15 hours at 70° C
  2. temperatureUpon cooling
  3. filtrationfiltered
  4. washwashed with methanol-water (1v/1v)
  5. customdried

出典と根拠

ORDレコード
ord-da4aacf49f5f45ad932b673d974757e6
出典データセット
uspto-grants-1976_12
特許番号
US04000146

反応ノート

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