反应详情

Triethylamine (1.8 mL, 13.2 mmol) was added to a cold (0° C.) solution of a mixture of the 2-(2,4,5-trifluorophenoxy)ethanol (1.3 g, 6.6 mmol; from Step 3) and methanesulfonyl chloride (0.61 mL, 7.9 mmol) in dichloromethane (40 mL). After being stirred for 1.5 h, water was added and the mixture was concentrated. The residue was dissolved in EtOAc and the solution was washed with 1 M KHSO4, then with brine, dried (Na2SO4) and concentrated to give 1.78 g (quantitative yield) of the title compound as an orange oil. NMR analysis supports the stated structure. This material was used directly in the next step.

1. concentrationthe mixture was concentrated
2. dissolutionThe residue was dissolved in EtOAc
3. washthe solution was washed with 1 M KHSO4
4. dry with materialwith brine, dried (Na2SO4)
5. concentrationconcentrated