反应详情

(2-Trifluoromethoxy-phenyl)-carbamic acid ethyl ester (42.4 g, 0.17 mol) was dissolved in THF (800 mL) and cooled to −70 ° C. sec-BuLi in cyclohexane (280 mL, 1.3 M) was added dropwise at this temperature with stirring. Stirring was continued for 1 h after addition was complete. A solution of iodine (43.2 g, 0.17 mol) in THF (160 mL) was added dropwise at −70 ° C. Stirring was continued for 1 h after addition was complete and the mixture was hydrolysed with saturated ammonium chloride solution. Water was added and the mixture was extracted with diethyl ether. The organic phases were washed with 40% sodium bisulfite, water, brine, pooled and dried with MgSO4. Evaporation of the solvent yielded the title compound, (60.2 g, 94%) as a colorless amorphous solid. (EI-MS: m/e=374.9 (M+))

1. additionwas added dropwise at this temperature
2. stirringStirring
3. additionafter addition
4. stirringStirring
5. waitwas continued for 1 h
6. additionafter addition
7. extractionthe mixture was extracted with diethyl ether
8. washThe organic phases were washed with 40% sodium bisulfite, water, brine
9. dry with materialdried with MgSO4
10. customEvaporation of the solvent