반응 #161869

반응 방정식

1-piperidin-4-yl-1,3-dihydroimidazo[4,5-b]pyridin-2-one

(2,6-dichloro-pyridin-4-yl)-(5-fluoro-2,3-dihydro-indol-1-yl)-methanone

DIPEA

→

1-[6′-chloro-4′-(5-fluoro-2,3-dihydro-indole-1-carbonyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl]-1,3-dihydro-imidazo[4,5-b]pyridin-2-one

용매

DMF

반응 조건

후처리

1. 1
   기타Then the reaction mixture was evaporated down
2. 2
   workup.ADDITIONthe residue was mixed with water
3. 3
   여과filtered
4. 4
   workup.STIRRINGstirred with diisopropylether and isopropanol and suction
5. 5
   여과filtered again
6. 6
   건조After drying the crude product
7. 7
   기타was purified by preparative HPLC-MS
8. 8
   기타freeze-dried

실험 절차

0.74 g (3.4 mmol) 1-piperidin-4-yl-1,3-dihydroimidazo[4,5-b]pyridin-2-one, 1.0 g (3.2 mmol) (2,6-dichloro-pyridin-4-yl)-(5-fluoro-2,3-dihydro-indol-1-yl)-methanone and 0.65 mL (3.8 mmol) DIPEA in 10 mL DMF were stirred for 2 h at RT. Then the reaction mixture was evaporated down, the residue was mixed with water and stirred for 30 min at RT. The precipitated solid was suction filtered, stirred with diisopropylether and isopropanol and suction filtered again. After drying the crude product was purified by preparative HPLC-MS. The product-containing fractions were combined and freeze-dried.

출처