반응 #2083

반응 방정식

3-methylxanthine

formaldehyde diethyl acetal

p-toluenesulfonyl chloride

sodium acetate

→

crude product

7-Ethoxymethyl-3-methylxanthine

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwere introduced
2. 2
   온도ice-cooling
3. 3
   workup.STIRRINGThe mixture was subsequently stirred for one hour
4. 4
   workup.STIRRINGagain subsequently stirred for one hour
5. 5
   온도After cooling to 10° C.
6. 6
   여과the precipitated product was filtered off with suction
7. 7
   세척washed with a little dimethylformamide
8. 8
   세척washed with demineralized water until chloride-free

실험 절차

52.5 g (0.28 mol) of p-toluenesulfonyl chloride were initially introduced into 50 ml of dimethylformamide and 22.6 g (0.29 mol) of sodium acetate were introduced with stirring and ice-cooling. The mixture was subsequently stirred for one hour, treated with 39.1 g of formaldehyde diethyl acetal and again subsequently stirred for one hour. 41.5 g of 3-methylxanthine were then introduced and the reaction mixture was heated at 90° C. for 2 hours. After cooling to 10° C., the precipitated product was filtered off with suction, washed with a little dimethylformamide and washed with demineralized water until chloride-free. The crude product obtained was recrystallized from dimethylformamide.

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