Reaktion #1810490

Reaktionsgleichung

hydrochloride

3-(1,3-dioxolan-2-yl)thiophene-2-sulfonamide

phenyl(4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate

1,8-diazabicyclo[5.4.0]undec-7-ene

→

product

Ausbeute 74.8%

3-(1,3-Dioxolan-2-yl)-N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl)aminocarbonyl]-2-thiophenesulfonamide

Ausbeute 74.8%

Lösungsmittel

water

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe resultant solution was extracted with methylene chloride
2. 2
   Trocknenthe methylene chloride phase was dried over magnesium sulfate
3. 3
   Filtrationfiltered
4. 4
   Sonstigeevaporated

Vorschrift

To 0.47 g of 3-(1,3-dioxolan-2-yl)thiophene-2-sulfonamide in 20 ml of acetonitrile was added 0.52 g of phenyl(4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate and 0.3 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). After stirring at ambient temperatures for two hours the solution was diluted to 50 ml with water and the pH was adjusted to 3 by the addition of hydrochloride acid. The resultant solution was extracted with methylene chloride and the methylene chloride phase was dried over magnesium sulfate, filtered and evaporated. Trituration of the residue with butyl chloride yielded 0.6 g of the product, m.p. 164°-166°. Infrared absorption spectra showed peaks at 1700, 1600 and 1550 cm-1, consistent for the desired structure. ##STR27##

Quelle