反应详情

10-[4-(2,2,2-Trifluoro-1-hydroxy-ethyl)-phenyl]-1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-9-one (402 mg, obtained in example 133, step 4) was dissolved in tetrahydrofuran (10 mL). Then, hydrochloric acid (2M, 5.22 mL) was added dropwise over a period of 10 minutes to the reaction mixture. The mixture was stirred for 3 hours at RT. The reaction mixture was poured into ice/water and was extracted two times with ethyl acetate. The combined organic layers were washed with brine, dried over Na2SO4, filtered and the solvent was evaporated. The residue was purified by flash chromatography (silica gel, gradient of heptane in ethyl acetate) to give the title compound as a colorless foam (265 mg, 73%). MS (m/e): 342.1 [MH+].

1. extractionwas extracted two times with ethyl acetate
2. washThe combined organic layers were washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was purified by flash chromatography (silica gel, gradient of heptane in ethyl acetate)