반응 #156452

반응 방정식

6-(6-Chloro-imidazo[1,2-b]pyridazin-3-ylmethyl)-7-fluoro-quinoline

KF

(rac)-methyl-pyrrolidin-3-yl-carbamic acid tert-butyl ester

→

title compound

(rac)-{1-[3-(7-fluoro-quinolin-6-ylmethyl)-imidazo[1,2-b]pyridazin-6-yl]-pyrrolidin-3-yl}-methyl-carbamic acid tert-butyl ester

용매

NMP

TBME

반응 조건

후처리

1. 1
   세척washed with water (3×)
2. 2
   추출The aqueous phases were further extracted with TBME (1×)
3. 3
   건조The combined organic layer was dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated in vacuo
6. 6
   기타The residue was crystallized in Et2O

실험 절차

6-(6-Chloro-imidazo[1,2-b]pyridazin-3-ylmethyl)-7-fluoro-quinoline (Stage 173.1, 150 mg, 0.474 mmol), KF (139 mg, 2.372 mmol) and (rac)-methyl-pyrrolidin-3-yl-carbamic acid tert-butyl ester (285 mg, 1.423 mmol) were suspended in NMP (1.5 mL). The RM was stirred at 170° C. for 1 h. The mixture was diluted with TBME and washed with water (3×). The aqueous phases were further extracted with TBME (1×). The combined organic layer was dried over Na2SO4, filtered and concentrated in vacuo. The residue was crystallized in Et2O to afford the title compound as a beige solid (tR 3.91 min (conditions 13), MH+=477).

출처