Pyridine, 2-methyl-4-nitro-, 1-oxide → HCID 178428516、化合物

HRID 358576

反応式

HRID 358576 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][N+:3]=1[O-:11]>CO.[Pd].C>[CH3:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N+:3]=1[O-:11]

参加物

4

反応物 1

HCID 95291Pyridine, 2-methyl-4-nitro-, 1-oxide

生成物 1

HCID 178428516HCID 178428516、化合物収率 96.2%

試薬・触媒・溶媒 2

HCID 14818447Palladiumcarbon触媒HCID 887Methanol溶媒

実験手順

4 g of 2-methyl-4-nitropyridine-N-oxide were dissolved in 90 ml of methanol and reduced with 1.2 g of 10% Pd/charcoal and H2. The catalyst was filtered off and the filtrate rotated in. The residue was boiled with 200 ml of ethyl acetate, filtered hot and the filtrate was mixed with 100 ml of hexane. The crystals precipitated after cooling the solution was sucked off, washed and dried. 3.1 g of 2-methyl-4-aminopyridine-N-oxide were obtained.

後処理

  1. filtrationThe catalyst was filtered off
  2. filtrationfiltered hot
  3. additionthe filtrate was mixed with 100 ml of hexane
  4. customThe crystals precipitated
  5. temperatureafter cooling the solution
  6. washwashed
  7. customdried

出典と根拠

ORDレコード
ord-89149ce471274d54bb86c6416d849b1f
出典データセット
uspto-grants-1991_03
特許番号
US04997835

関連ノート

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