反应详情

A reaction vessel was charged with lithiumaluminium hydride (23.5 mg, 0.618 mmol) and dry tetrahydrofuran (1 mL). N-[2-({1-[1-(4-fluorophenyl)cyclobutyl]-2-nitroso-1,2,3,4-tetrahydroisoquinolin-7-yl}oxy)ethyl]propane-1-sulfonamide (49 mg, 0.103 mmol, cf. example 75) was added dropwise as a solution in dry tetrahydrofuran (1 mL) at 0° C. After the addition was completed the reaction mixture was stirred at room temperature for 1 h and then at 40-50° C. for 1 h. After cooling to room temperature the reaction mixture was poured on ice water (15 mL) and the aqueous phase was extracted with ethyl acetate (3×10 mL). The combined extracts were dried (MgSO4) and concentrated in vacuo. The crude product was purified by preparative HPLC (RP, acetonitrile, water). Yield: 1 mg (2.2 μmol, 2%).

1. additionAfter the addition
2. waitat 40-50° C. for 1 h
3. temperatureAfter cooling to room temperature the reaction mixture
4. additionwas poured on ice water (15 mL)
5. extractionthe aqueous phase was extracted with ethyl acetate (3×10 mL)
6. dry with materialThe combined extracts were dried (MgSO4)
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by preparative HPLC (RP, acetonitrile, water)