Reaktion #451806

Reaktionsgleichung

2-mercapto-3-allyl-4(3H)-quinazolinone

product

2-mercapto-3-allyl-4(3H)-quinazolinone

chloromethyl thiocyanate

sodium hydride

→

2-Thiocyanomethyl-3-allyl-4(3H)-quinazolinone

Lösungsmittel

dimethoxyethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed at 50° C. for 8 hours
2. 2
   workup.STIRRINGstirred overnight
3. 3
   Temperaturrefluxed at 50° C. for 8 hours
4. 4
   workup.STIRRINGstirred overnight
5. 5
   WaschenThe reaction mixture was washed with water
6. 6
   Extraktionextracted with methylene chloride
7. 7
   Trocknendried over magnesium sulfate
8. 8
   SonstigeThe oily residue was triturated with ether
9. 9
   Sonstigeto give the above-identified product

Vorschrift

To a mixture of 5.8 g (0.03 mole) 2-mercapto-3-allyl-4(3H)-quinazolinone (the product of Example 5) in 200 ml dimethoxyethane, 5.4 g (0.05 mole) chloromethyl thiocyanate and 2.4 g (0.05 mole) 50% sodium hydride were added. The resulting mixture was stirred overnight at ambient temperature, refluxed at 50° C. for 8 hours, stirred overnight, refluxed at 50° C. for 8 hours and stirred overnight. The reaction mixture was washed with water, extracted with methylene chloride, dried over magnesium sulfate and stripped. The oily residue was triturated with ether, to give the above-identified product, as a solid, melting point 73°-76° C.

Quelle