Reaktion #441823

Reaktionsgleichung

hydrochloric acid

N-methylsaccharin

N-(2-pyridyl)chloroacetamide

sodium hydride

→

4-hydroxy-2-methyl-N-2-pyridyl-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas then added to 100 ml
2. 2
   FiltrationThe precipitate was filtered
3. 3
   Sonstigedried
4. 4
   Sonstigeto give 24 mg

Vorschrift

To a solution of 590 mg. (3 mmole) of N-methylsaccharin and 1.02 g. (6 mmole) of N-(2-pyridyl)chloroacetamide in 3 ml. of dimethylformamide at 40° C. was added 250 mg. (10.3 mmole) of 99% sodium hydride portionwise over a period of one hour. The reaction mixture was allowed to stir at 40° C. for 2.5 hours and was then added to 100 ml. of 5% hydrochloric acid solution and 300 ml. of ice. The precipitate was filtered and dried to give 24 mg.

Quelle