2-Amino-3-nitro-5-(2-methylpropyl)pyridine → 2,3-Diamino-5-(2-methylpropyl)pyridine

HRID 722053ノート

反応式

HRID 722053 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([CH2:11][CH:12]([CH3:14])[CH3:13])=[CH:4][N:3]=1>CO.[Pd]>[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([CH2:11][CH:12]([CH3:14])[CH3:13])=[CH:4][N:3]=1

参加物

4

反応物 1

HCID 218827302-Amino-3-nitro-5-(2-methylpropyl)pyridine2 回

生成物 1

HCID 218827102,3-Diamino-5-(2-methylpropyl)pyridine収率 87.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

0.46 g of 2-amino-3-nitro-5-(2-methylpropyl)pyridine (starting material D2) dissolved in 20 ml of methanol are hydrogenated over 0.05 g of 10% strength Pd/C until no starting material is detectable by TLC. After filtration, the solvent is evaporated and the residue is chromatographed over silica gel (dichloromethane/methanol 25:1). Concentration of the pure fractions and drying in vacuo gives 0.34 g of the title compound as an oil. The mass spectrum shows the molecular peak MH+ at 166.2 Da.

後処理

  1. filtrationAfter filtration
  2. customthe solvent is evaporated
  3. customthe residue is chromatographed over silica gel (dichloromethane/methanol 25:1)
  4. customConcentration of the pure fractions and drying in vacuo

出典と根拠

ORDレコード
ord-e28a9d04c2e443f0bf6b24b53ff96b7c
出典データセット
uspto-grants-2006_11
特許番号
US07138399B2

反応ノート

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