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Phosphoric Acid → HCID 178428356, Verbindung

HRID 1728574
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1728574
[CH:1]1([C:4](O)=O)[CH2:3][CH2:2]1.P(=O)(O)(O)O.[NH2:12][C:13]1[C:18]([NH2:19])=[C:17]([CH3:20])[CH:16]=[CH:15][N:14]=1.[OH-].[K+]>O>[CH:1]1([C:4]2[NH:12][C:13]3=[N:14][CH:15]=[CH:16][C:17]([CH3:20])=[C:18]3[N:19]=2)[CH2:3][CH2:2]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1004Phosphoric AcidHCID 14797Potassium HydroxideHCID 15655Cyclopropanecarboxylic acidHCID 3174954-Methylpyridine-2,3-diamine

Produkt 1

HCID 178428356HCID 178428356, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

30 ml of cyclopropanecarboxylic acid and 70 ml of phosphoric acid (85%) were added to 15 g of 2,3-diamino-4-methylpyridine, and the mixture was stirred at an internal temperature of 130° C. for 12 hr. The reaction mixture was cooled, poured into a solution of 140 g of potassium hydroxide in 420 ml of water and then extracted with chloroform. The extract was dried over anhydrous magnesium sulfate and then concentrated. The residue was purified by column chromatography (chloroform:ethanol=97:3). The yield was 14.1 g, and the product was recrystallized from ethyl acetate-isopropyl ether to prepare the title compound in a pure form having a melting point of 203° to 204° C.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with chloroform
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography (chloroform:ethanol=97:3)
  6. customThe yield was 14.1 g, and the product was recrystallized from ethyl acetate-isopropyl ether
  7. customto prepare the title compound in a pure form

Quellen und Nachweise

ORD-Eintrag
ord-a63b072eeb0c4bb28d9c0fcf2e0f4e29
Quelldatensatz
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05328911

Notizen zur Reaktion

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