Methanol → 2,6-Dianilino-3,5-dinitropyridine

HRID 267498

反応式

HRID 267498 の反応式
[N+:1]([C:4]1[C:5](CS(N)(=O)=O)=[N:6][C:7](CS(N)(=O)=O)=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)([O-:3])=[O:2].[NH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C[N:31](C)[C:32](=O)[CH3:33].CO>C(N(CC)CC)C>[NH:23]([C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][C:8]([N+:10]([O-:12])=[O:11])=[C:7]([NH:31][C:32]2[CH:33]=[CH:8][CH:9]=[CH:4][CH:5]=2)[N:6]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

6

反応物 4

HCID 887MethanolHCID 6115AnilineHCID 31374DimethylacetamideHCID 215548863,5-Dinitro-2,6-pyridine dimethanesulfonamide

生成物 1

HCID 215548872,6-Dianilino-3,5-dinitropyridine収率 70%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
140 °C

実験手順

Under a nitrogen atmosphere, a mixture of 3,5-dinitro-2,6-pyridine dimethanesulfonamide (50 g, 0.14 mole), 200 ml aniline and 250 ml N,N-dimethylacetamide was heated with stirring to 140°C and then maintained at this temperature for 6 hours. The warm (90°C) mixture was poured onto 450 ml methanol with stirring and 20 ml triethylamine added. The precipitate was washed with methanol and dried to afford 2,6-dianilino-3,5-dinitropyridine (34.5 g, 70%) as an orange solid, mp. 224-225.5. Anal. Calcd. for C17H13N5O4 : C, 58.1; H, 3.7. Found: c, 57.4; H, 3.4.

後処理

  1. temperaturewas heated
  2. temperaturemaintained at this temperature for 6 hours
  3. temperatureThe warm (90°C) mixture
  4. stirringwith stirring
  5. washThe precipitate was washed with methanol
  6. customdried

出典と根拠

ORDレコード
ord-a59b774f77aa449f9522037a32e3fe9e
出典データセット
uspto-grants-1976_03
特許番号
US03943125

関連ノート

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