반응 #157267

반응 방정식

{2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidin-4-yl}-(3-morpholin-4-ylmethyl-phenyl)-amine

hydrogen peroxide

ammonia

→

product

{2-[4-(4-chloro-phenyl)-piperazin-1-yl]-5-oxo-6,7-dihydro-5H-5λ4-thieno[3,2-d]pyrimidin-4-yl}-(3-morpholin-ylmethyl-phenyl)-amine

용매

acetic acid

—

ice water

반응 조건

후처리

1. 1
   기타The precipitate formed
2. 2
   여과filtered
3. 3
   세척washed with water
4. 4
   기타dried
5. 5
   추출The crude product is extracted with petroleum ether and diethyl ether, suction
6. 6
   여과filtered
7. 7
   기타dried
8. 8
   기타The product is purified by chromatography (10 g Chromabond SiOH-cartridge)

실험 절차

313.80 mg {2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidin-4-yl}-(3-morpholin-4-ylmethyl-phenyl)-amine are placed in 2.70 ml glacial acetic acid and cooled to 10° C. 57 μl hydrogen peroxide (35%) are added dropwise, then the mixture is stirred for 0.25 hours. Then the reaction mixture is stirred in 30 ml ice water and made basic with cold ammonia solution. The precipitate formed is suction filtered, washed with water and dried. The crude product is extracted with petroleum ether and diethyl ether, suction filtered and dried. The product is purified by chromatography (10 g Chromabond SiOH-cartridge). 140.0 mg of the product are obtained as a powder (m.p 244°-248° C.).

출처