Methanesulfonic Acid → 3,5-Diamino-2,6-di(methylamino)pyridine

HRID 267499

反応式

HRID 267499 の反応式
[CH3:1][NH:2][C:3]1[C:8]([N+:9]([O-])=O)=[CH:7][C:6]([N+:12]([O-])=O)=[C:5]([NH:15][CH3:16])[N:4]=1.CS(O)(=O)=O.[H][H]>[Pd].C.CO>[NH2:9][C:8]1[C:3]([NH:2][CH3:1])=[N:4][C:5]([NH:15][CH3:16])=[C:6]([NH2:12])[CH:7]=1

参加物

6

反応物 3

HCID 6395Methanesulfonic AcidHCID 21554890HCID 21554890、化合物HCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 203634173,5-Diamino-2,6-di(methylamino)pyridine

試薬・触媒・溶媒 2

HCID 14818447Palladiumcarbon触媒HCID 887Methanol溶媒

実験手順

A 250 ml Parr bottle was charged with 2,6-di(methylamino)-3,5-dinitropyridine (20.0 g, 0.088 mole), 30 ml methanesulfonic acid, 200 ml methanol and 1.0 g 5% Pd/charcoal catalyst. The mixture was subjected to hydrogenation at ambient temperature with an initial hydrogen pressure of 65 psig. When no further uptake of hydrogen was observed, the mixture was treated with anhydrous silica gel (25 g), filtered free of catalyst and drying agent under a nitrogen atmosphere, and methanol removed under vacuum. The trimethanesulfonate salt of 3,5-diamino-2,6-di(methylamino)pyridine was obtained under nitrogen by addition of cold i-butanol-benzene to the concentrate, followed by vacuum drying (40°-50°C) over P2O5.

後処理

  1. additionthe mixture was treated with anhydrous silica gel (25 g)
  2. filtrationfiltered free of catalyst
  3. customdrying agent under a nitrogen atmosphere
  4. custommethanol removed under vacuum

出典と根拠

ORDレコード
ord-20dcc80e347542b598402949fe9e27c7
出典データセット
uspto-grants-1976_03
特許番号
US03943125

関連ノート

読み込み中…