反应详情

Sodium hydride (0.626 g, 15.64 mmol, 60% suspension in mineral oil) was washed under dry conditions under nitrogen atmosphere with n-hexane. Dimethylformamide (20 mL) was added followed by 1-[1-(4-fluorophenyl)cyclobutyl]-3,4-dihydroisoquinolin-7-ol (2.1 g, 7.11 mmol) under stirring. After the exothermic reaction had ceased stirring was continued at room temperature for 1 h before tert-butyl (2-bromoethyl)carbamate (4.78 g, 21.33 mmol) was added dropwise as a solution in dimethylformamide (10 mL). The reaction mixture was stirred at room temperature over night. The solvent was evaporated in vacuo. Ice water was added (60 mL) and the aqueous phase was extracted with ethyl acetate. The combined organic layers were dried (MgSO4) and the solvent was evaporated in vacuo.

1. customAfter the exothermic reaction
2. stirringhad ceased stirring
3. stirringThe reaction mixture was stirred at room temperature over night
4. customThe solvent was evaporated in vacuo
5. additionIce water was added (60 mL)
6. extractionthe aqueous phase was extracted with ethyl acetate
7. dry with materialThe combined organic layers were dried (MgSO4)
8. customthe solvent was evaporated in vacuo