Reaktion #570996

Reaktionsgleichung

7-hydroxy-3,4-dimethylcoumarin

2-chloromethyl-5-methyl-1,3,4-thiadiazole

K2CO3

→

3,4-Dimethyl-7-(2-methyl-1,3,4-thiadiazol-5-yl)-methoxycoumarin

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 20 hours
2. 2
   Sonstigeevaporated down
3. 3
   Sonstigethe residue was partitioned in H2O/methylene chloride
4. 4
   SonstigeAfter the undissolved constituents had been separated off
5. 5
   Waschenthe organic phase was washed once with 1 N NaOH
6. 6
   Trocknenwith H2O, dried over Na2SO4
7. 7
   Sonstigeevaporated down
8. 8
   Sonstigethe residue was recrystallized from methanol
9. 9
   Sonstigedried

Vorschrift

A mixture of 5.0 g of 7-hydroxy-3,4-dimethylcoumarin, 3.9 g of 2-chloromethyl-5-methyl-1,3,4-thiadiazole, 3.5 g of K2CO3 and 100 ml of acetone was refluxed for 20 hours and evaporated down, and the residue was partitioned in H2O/methylene chloride. After the undissolved constituents had been separated off, the organic phase was washed once with 1 N NaOH and then with H2O, dried over Na2SO4 and evaporated down, and the residue was recrystallized from methanol and dried.

Quelle