반응 #82526

반응 방정식

2,4-diamino-6-methylpyrimidine

iodine monochloride

sodium hydroxide

→

2,4-diamino-5-iodo-6-methylpyrimidine

수율 73.1%

용매

water

acetic acid

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONUpon completion of addition
2. 2
   추출The mixture is then extracted with three 75 mL portions of ethyl acetate
3. 3
   세척The combined extracts are washed with one 75 mL portion of an aqueous solution saturated with sodium chloride
4. 4
   건조The organic layer is dried with sodium sulfate
5. 5
   여과filtered
6. 6
   농축The filtrate is concentrated under reduced pressure

실험 절차

A solution of 8.0 grams (0.064 mole) of 2,4-diamino-6-methylpyrimidine in 30 mL of glacial acetic acid is stirred, and a solution of 13.5 grams (0.083 mole) of iodine monochloride in 20 mL of glacial acetic acid is added dropwise during a 5 minute period. Upon completion of addition, the reaction mixture is stirred at ambient temperature for about 18 hours. After this time the reaction mixture is diluted with 100 mL of water and then is made basic with 10% aqueous sodium hydroxide. The mixture is then extracted with three 75 mL portions of ethyl acetate. The combined extracts are washed with one 75 mL portion of an aqueous solution saturated with sodium chloride. The organic layer is dried with sodium sulfate and filtered. The filtrate is concentrated under reduced pressure, yielding 11.7 grams of 2,4-diamino-5-iodo-6-methylpyrimidine. The NMR spectrum is consistent with the proposed structure.

출처