Ammonia → HCID 16426513, Verbindung

HRID 2206843Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2206843
[Cl:1][C:2]1[C:3]([C:10](Cl)=[O:11])=[N:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1.[NH3:13].O>O1CCOCC1.CO>[Cl:1][C:2]1[C:3]([C:10]([NH2:13])=[O:11])=[N:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1

Komponenten

6

Edukt 3

HCID 222AmmoniaHCID 962WaterHCID 140671885-Chloro-2-(methylsulfanyl)pyrimidine-4-carbonyl chloride

Produkt 1

HCID 16426513HCID 16426513, VerbindungAusbeute 53 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

15 g (67.2 mmol) of 5-chloro-2-(methylsulfanyl)pyrimidine-4-carbonyl chloride are dissolved in 35 ml of dioxane and cooled to 5° C. 57.3 g (0.4 mol) of 7N ammonia in methanol (about 12% strength solution) are slowly added dropwise to the cooled solution. During the addition, the reaction temperature was kept below 15° C. After the dropwise addition had ended, the reaction mixture was allowed to warm to room temperature and stirred for about 15 hours. The mixture was then added to water and the precipitated 5-chloro-2-(methylsulfanyl)pyrimidine-4-carboxamide was isolated (7.7 g, yield 53% at a purity of 95%).

Aufarbeitung

  1. additionDuring the addition
  2. customwas kept below 15° C
  3. additionAfter the dropwise addition
  4. temperatureto warm to room temperature

Quellen und Nachweise

ORD-Eintrag
ord-0c7c34a76b774d5ea75187e804e921d9
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09375002B2

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