반응 #157270

반응 방정식

2,4-dichloro-6,7-dihydro-thieno[3,2-d]pyrimidine

diisopropylethylamine

3-fluoro-aniline

→

product

(2-chloro-6,7-dihydro-thieno[3,2-d]pyrimidin-4-yl)-(3-fluoro-phenyl)-amine

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도after cooling
2. 2
   기타evaporated down
3. 3
   추출The residue is extracted with dichloromethane and water
4. 4
   세척the organic phase is washed with saturated sodium chloride solution
5. 5
   기타dried
6. 6
   기타evaporated to dryness
7. 7
   기타The residue is purified by chromatography (NP_MPLC, Biotage cartridge (4*15 cm))

실험 절차

4.00 g 2,4-dichloro-6,7-dihydro-thieno[3,2-d]pyrimidine are placed in 15 ml dimethylformamide, then first 4.50 ml diisopropylethylamine, then 2.50 ml 3-fluoro-aniline are added. The reaction mixture is stirred for 7 hours at 120° C., and after cooling evaporated down. The residue is extracted with dichloromethane and water, the organic phase is washed with saturated sodium chloride solution, dried and evaporated to dryness. The residue is purified by chromatography (NP_MPLC, Biotage cartridge (4*15 cm)). 2.60 g of the product are obtained as a powder.

출처