反应详情

A solution of 2,2,2-trichloroethanol (2.46 g, 16.5 mmol) and NEt3 (1.67 g, 16.5 mmol) in CH2Cl2 (40 ml) at 0° C. was dropwise added 4-bromomethyl benzoylbromide (4.17 g, 15.0 mmol) in CH2Cl2 (20 ml) and stirred to room temperature overnight. The reaction mixture was added H2O (20 ml) and the organic layer separated. The organic layer washed with aqueous 1 M HCl (20 ml) and H2O (20 ml). The organic layer was dried over Na2SO4, filtered and the solvent evaporated in vacuo to leave the expected product as a white solid. The product was used directly in the next step without any further purification (to be filled in).

1. customat 0° C.
2. customthe organic layer separated
3. washThe organic layer washed with aqueous 1 M HCl (20 ml) and H2O (20 ml)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customthe solvent evaporated in vacuo