反应详情

To 6.3 g of N-[6-(hydroxymethyl)-1-isoquinolinyl]benzamide (1 g) in 40 mL of toluene and 40 mL of dioxane at 0° C. 7.8 mL of diphenylphosphoryl azide (DDPA) and 5.4 mL of 1,8-diazabicyclo(5.4.0)undec-7ene (DBU) were added. After 24 hours the reaction mixture was poured into water (pH 7) and extracted with ethyl acetate. The organic layer was dried (sodium sulfate) and concentrated. Trituration with diethyl ether gave 6.4 g of the title compound. Mp. 125-129° C. MS (m/e)=303.

1. customat 0° C
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried (sodium sulfate)
4. concentrationconcentrated