반응 #1486348

반응 방정식

1-[9-chloro-1-(2-chloro-4-methoxyphenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propan-1-ol

acetic anhydride

→

title compound

수율 70.0%

1-[9-Chloro-1-(2-chloro-4-methoxyphenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propyl acetate

수율 70.0%

용매

pyridine

반응 조건

후처리

1. 1
   농축The mixture was concentrated
2. 2
   추출extracted with ethyl acetate (×3)
3. 3
   세척The combined organic layer was washed with brine (×1)
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo
7. 7
   기타The residue was purified by silica gel column chromatography
8. 8
   세척eluting with a 0-40% ethyl acetate/n-hexane gradient mixture
9. 9
   기타The residue was recrystallized from methanol/n-hexane

실험 절차

To a solution of 1-[9-chloro-1-(2-chloro-4-methoxyphenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propan-1-ol (122.0 mg, 0.300 mmol) in pyridine (0.5 mL) was added acetic anhydride (0.5 mL) at 0° C. The reaction mixture was stirred at room temperature for 5 hrs. The mixture was concentrated. The residue was neutralized with aqueous saturated sodium hydrogen carbonate and extracted with ethyl acetate (×3). The combined organic layer was washed with brine (×1), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 0-40% ethyl acetate/n-hexane gradient mixture. The residue was recrystallized from methanol/n-hexane to give the title compound as a colorless powder (94.7 mg, 0.211 mmol, 70%).

출처