반응 #1486288

반응 방정식

Lithium borohydride

methyl 9-chloro-1-(2-methoxy-4,6-dimethylpyrimidin-5-yl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carboxylate

→

title compound

수율 98.0%

[9-Chloro-1-(2-methoxy-4,6-dimethylpyrimidin-5-yl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]methanol

수율 98.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   기타The reaction was quenched by methanol
2. 2
   workup.ADDITIONthe mixture was diluted with aqueous saturated ammonium chloride at 0° C
3. 3
   추출The mixture was extracted with tetrahydrofuran/ethyl acetate
4. 4
   세척The combined organic layer was washed with brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated in vacuo
8. 8
   세척The residue was washed with ethyl acetate/diisopropyl ether

실험 절차

Lithium borohydride (1.93 g, 88.4 mmol) was added to a stirred solution of methyl 9-chloro-1-(2-methoxy-4,6-dimethylpyrimidin-5-yl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carboxylate (8.87 g, 22.1 mmol) in tetrahydrofuran (100 mL) at room temperature, and the mixture was stirred at 40° C. for 14 hr. The reaction was quenched by methanol, and the mixture was diluted with aqueous saturated ammonium chloride at 0° C. The mixture was extracted with tetrahydrofuran/ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was washed with ethyl acetate/diisopropyl ether to give the title compound as a colorless powder (8.08 g, 21.6 mmol, 98%).

출처