3,4-Diaminopyridine → HCID 178503896, Verbindung

HRID 257423

Reaktionsgleichung

Reaktionsgleichung von HRID 257423
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8].[CH3:9][S:10][C:11](SC)=[N:12][C:13]#[N:14]>N1C=CC=CC=1>[CH3:9][S:10][C:11](=[N:12][C:13]#[N:14])[NH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8]

Komponenten

4

Edukt 2

HCID 59183,4-DiaminopyridineHCID 66289Dimethyl N-cyanodithioiminocarbonate

Produkt 1

HCID 178503896HCID 178503896, VerbindungAusbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

3,4-Diaminopyridine (4 g, 36.6 mmol) was suspended in anhydrous pyridine (100 ml), and S,S'-dimethyl N-cyanodithioiminocarbonate (8.0 g, 55.0 mmol) was added thereto. The mixture was stirred at room temperature for 4 days. The resulting powder was collected from the reaction mixture by filtration, and washed with ether (100 ml) to obtain crude crystals. The crystals were purified by recrystallization from methanol-ether to obtain 1.91 g of the intended product as a white powder (yield: 58%). On the other hand, the filtrate was concentrated under reduced pressure, and the residue was purified by flash column chromatography (silica gel, eluent: chloroform:methanol=4:1 (v/v)) to obtain 2.8 g of the intended product (total yield: 95%).

Aufarbeitung

  1. filtrationThe resulting powder was collected from the reaction mixture by filtration
  2. washwashed with ether (100 ml)
  3. customto obtain crude crystals
  4. customThe crystals were purified by recrystallization from methanol-ether

Quellen und Nachweise

ORD-Eintrag
ord-9cb7892e7c7344dfae5c4dd0d1699a69
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05262415

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