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Methanesulfonic Acid → HCID 19012219, 화합물

HRID 1974019
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HRID 1974019 반응식
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([CH3:11])[C:5]([N+:12]([O-])=O)=[C:4]([CH3:15])[N:3]=1.CS(O)(=O)=O.[H][H]>[Pd].C.CO>[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([CH3:11])[C:5]([NH2:12])=[C:4]([CH3:15])[N:3]=1
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참가 물질

6

반응물 3

HCID 6395Methanesulfonic AcidHCID 197540694,6-Dimethyl-3,5-dinitropyridin-2-amineHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 19012219HCID 19012219, 화합물

시약·촉매·용매 2

HCID 14818447Palladiumcarbon촉매HCID 887Methanol용매

실험 절차

A 500 ml Parr Bottle was charged with 2-amino-4,6-dimethyl-3,5-dinitropyridine (21.2 g, 0.10 mole), 200 ml methanol, methanesulfonic acid (19.2 g, 0.20 mole), and 20. g 5% Pd/charcoal catalyst. The mixture was subjected to hydrogenation at ambient temperature with an initial hydrogen pressure of 5.7 psig. When no further uptake of hydrogen was observed, the mixture was filtered free of catalyst under a nitrogen atmosphere, and methanol removed under vacuum. The bismethanesulfonate salt of 2,3,5-triamino-4,6-dimethylpyridine so obtained was purified by slurrying with dry isopropyl alcohol, filtering under nitrogen, and vacuum drying over P2O5 at 80° - 90° C.

후처리

  1. filtrationthe mixture was filtered free of catalyst under a nitrogen atmosphere
  2. custommethanol removed under vacuum

출처 및 근거

ORD 기록
ord-249859c417384553bdaa621540d9c40a
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04000146

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