反応 #451806

反応方程式

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

溶媒

dimethoxyethane

反応条件

後処理

1. 1
   温度refluxed at 50° C. for 8 hours
2. 2
   workup.STIRRINGstirred overnight
3. 3
   温度refluxed at 50° C. for 8 hours
4. 4
   workup.STIRRINGstirred overnight
5. 5
   洗浄The reaction mixture was washed with water
6. 6
   抽出extracted with methylene chloride
7. 7
   乾燥dried over magnesium sulfate
8. 8
   その他The oily residue was triturated with ether
9. 9
   その他to give the above-identified product

実験手順

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.

出典