反应详情

To a solution of NaOH (47.2 g, 1.18 mole) in ice/H2O (270 g) maintained at 4°-5° C. was added Br2 (68.7 g, 0.43 mole) followed by 4-methyl-4-phenyl-2-pentanone (23.7 g, 0.135 mole). The reaction was stirred for 18 hours at room temperature. The crude reaction mixture was extracted with CCl4 (discarded), acidified to pH 1-2 with concentrated HCl solution and extracted with ethyl acetate. The combined organics were washed with saturated NaCl solution, dried over Na2SO4 and evaporated in vacuo to obtain 22.5 g of the title B compound as an off-white solid. This was used in the next step without further purification. MS: (M+NH4)+ @ 196.

1. customThe crude reaction mixture
2. extractionwas extracted with CCl4 (discarded)
3. extractionextracted with ethyl acetate
4. washThe combined organics were washed with saturated NaCl solution
5. dry with materialdried over Na2SO4
6. customevaporated in vacuo
7. customto obtain 22.5 g of the title B compound as an off-white solid
8. customThis was used in the next step without further purification