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Acetyl chloride → N-(4,6-Dichloropyrimidin-2-yl)acetamide

HRID 1730144
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1730144
C(O[C:5](=[O:7])[CH3:6])(=O)C.[NH2:8][C:9]1[N:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[N:10]=1.C(Cl)(=O)C>>[C:5]([NH:8][C:9]1[N:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[N:10]=1)(=[O:7])[CH3:6]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 6367Acetyl chlorideHCID 7918Acetic AnhydrideHCID 655222-Amino-4,6-dichloropyrimidine

Produkt 1

HCID 12611964N-(4,6-Dichloropyrimidin-2-yl)acetamide

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A 250 ml. three necked flask was fitted with a mechanical stirrer and a reflux condenser with drying tube. The flask is charged with 50 ml. of acetic anhydride and 3.85 g of 2-amino-4,6-dichloropyrimidine (0.025 mole). Then, 10 ml. of acetyl chloride was added slowly and the mixture was heated to 110° C for 8 hours. The mixture was allowed to stand overnight at room temperature. The crystalline solid product which formed was filtered and washed with water and sodium bicarbonate solution. It was then recrystallized from 50% alcohol. There was obtained 3.8 g of 2-acetamido-4,6-dichloropyrimidine (PY-25) in the form of white crystals, melting point, 198°-200° C, yield, 74.5%.

Aufarbeitung

  1. customthree necked flask was fitted with a mechanical stirrer and a reflux condenser
  2. customwith drying tube
  3. additionThe flask is charged with 50 ml
  4. customThe crystalline solid product which formed
  5. filtrationwas filtered
  6. washwashed with water and sodium bicarbonate solution
  7. customIt was then recrystallized from 50% alcohol

Quellen und Nachweise

ORD-Eintrag
ord-d9a1175b5f344b87b702f550625511ad
Quelldatensatz
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03991190

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