反应详情

TMSCN (0.14 mL, 1.01 mmol) was added to a mixture of the compound 68 (60 mg, 0.34 mmol), cyclobutanone (0.15 mL, 2.04 mmol) and ZnCl2 (4 mg, 0.04 mmol) in dioxane (1 mL) with stirring. The reaction mixture was stirred at room temperature for 1 h, and concentrated in vacuo. The residue was diluted with water, and extracted with DCM. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated to dryness to give compound 70 (80 mg, 91%) as a light yellow oil. The crude product was used directly for the next step without purification.

1. stirringThe reaction mixture was stirred at room temperature for 1 h
2. concentrationconcentrated in vacuo
3. additionThe residue was diluted with water
4. extractionextracted with DCM
5. washThe combined organic layers were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated to dryness