반응 #80910

반응 방정식

1,4-diazabicyclo(2,2,2)octane

2,4-diamino-6-(3,4-dichlorophenylthio)quinazoline

ammonium hydroxide

→

2,4-diamino-6-(3,4-dichlorophenylsulfinyl)quinazoline

용매

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONUpon completion of addition
2. 2
   workup.STIRRINGthe reaction mixture was stirred at ambient temperature for about 20 hours
3. 3
   여과The resultant solid was collected by filtration
4. 4
   기타triturated with methanol
5. 5
   여과The solid was collected by filtration
6. 6
   기타dried

실험 절차

A suspension of 5.0 grams (0.011 mole) of the bromine complex of 1,4-diazabicyclo(2,2,2)octane in 200 mL of aqueous 70% acetic acid was stirred, and 3.4 grams (0.01 mole) of 2,4-diamino-6-(3,4-dichlorophenylthio)quinazoline was added portionwise during about a 1 hour period. Upon completion of addition, the reaction mixture was stirred at ambient temperature for about 20 hours. After this time, the reaction mixture was neutralized with concentrated ammonium hydroxide. The resultant solid was collected by filtration and triturated with methanol. The solid was collected by filtration and dried, yielding 2,4-diamino-6-(3,4-dichlorophenylsulfinyl)quinazoline, mp 200° C., dec. The NMR spectrum was consistent with the proposed structure.

출처