반응 #162203

반응 방정식

3-[[2-[5-chloro-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridin-3-yl]-5-fluoro-pyrimidin-4-yl]amino]-2-hydroxy-cyclohexanecarboxylic acid

65b

3-[[2-[5-chloro-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridin-3-yl]-5-fluoro-pyrimidin-4-yl]amino]-2-hydroxy-cyclohexanecarboxylic acid

iPr2NEt

ethanamine hydrochloride

HATU

→

3-[[2-[5-chloro-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridin-3-yl]-5-fluoro-pyrimidin-4-yl]amino]-N-ethyl-2-hydroxy-cyclohexanecarboxamide

용매

EtOAc

DMF

반응 조건

후처리

1. 1
   세척the mixture was washed with 1 N HCl, aqueous saturated NH4Cl solution, and brine
2. 2
   건조The organic phase was dried over Na2SO4
3. 3
   여과filtered
4. 4
   농축concentrated in vacuo
5. 5
   기타The crude product was used in the next step without further purification

실험 절차

3-[[2-[5-chloro-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridin-3-yl]-5-fluoro-pyrimidin-4-yl]amino]-2-hydroxy-cyclohexanecarboxylic acid, 65b, (0.100 g, 0.179 mmol) was dissolved in DMF (2 mL) and iPr2NEt (0.124 mL, 0.714 mmol) and ethanamine hydrochloride (0.029 g, 0.357 mmol) was added at room temperature. Then HATU (0.081 g, 0.214 mmol) was added to the solution at room temperature. After 30 min, EtOAc was added and the mixture was washed with 1 N HCl, aqueous saturated NH4Cl solution, and brine. The organic phase was dried over Na2SO4, filtered and concentrated in vacuo. The crude product was used in the next step without further purification.

출처