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Hydrochloric Acid → HCID 19012219, 화합물

HRID 2397587
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HRID 2397587 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.C(O)C.[H][H].Cl>[Pd].C.C(O)(C)C>[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

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 197540694,6-Dimethyl-3,5-dinitropyridin-2-amineHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 19012219HCID 19012219, 화합물

시약·촉매·용매 2

HCID 14818447Palladiumcarbon촉매
HCID 3776
Isopropanol
용매

실험 절차

A 500 ml Parr Bottle was charged with 2-amino-4,6-dimethyl-3,5-dinitropyridine (21.2 g, 0.10 mole), 250 ml absolute ethanol, and 20 g 5% Pd/charcoal catalyst. The mixture was subjected to hydrogenation at ambient temperature with an initial hydrogen pressure of 60 psig. When no further uptake of hydrogen was observed, the mixture was filtered free of catalyst under a nitrogen atmosphere, and concentrated under vacuum to a volume of about 100 ml. The product concentrate was treated, under nitrogen at ice temperature, with a cold solution of hydrogen chloride (0.5 mole) in 85 ml anhydrous isopropyl alcohol. The trihydrochloride salt of 2,3,5-triamino-4,6-dimethylpyridine was obtained after vigorous stirring, filtering under nitrogen, and vacuum drying under high vacuum over P2O5 at 80°-90° C.

후처리

  1. filtrationthe mixture was filtered free of catalyst under a nitrogen atmosphere
  2. concentrationconcentrated under vacuum to a volume of about 100 ml
  3. concentrationThe product concentrate

출처 및 근거

ORD 기록
ord-2a56b0bd65d64252a834100e2697cee7
출처 데이터셋
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04022793

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