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

HRID 267499

반응식

HRID 267499 반응식
[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

참가 물질

6

반응물 3

HCID 6395Methanesulfonic AcidHCID 21554890HCID 21554890, 화합물HCID 178418361HCID 178418361, 화합물2회

생성물 1

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

시약·촉매·용매 2

HCID 14818447Palladiumcarbon촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-20dcc80e347542b598402949fe9e27c7
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03943125

연결된 노트

불러오는 중…