反应详情

Methyl magnesium iodide (3M solution in diethyl ether, 0.17 mL, 0.522 mmol, 1.5 eq) was added at −70° C. to a stirred solution of 28a) (150 mg, 0.348 mmol, 1.0 eq) in dry THF (10 mL) and stirring was continued for 2 h at −50° C. The reaction mixture was quenched with ammonium chloride solution, diluted with water (20 mL), and extracted with ethyl acetate (2×20 mL). The organic layers were washed with brine, dried over sodium sulfate, and evaporated. The residue was purified by preparative TLC using 70% ethyl acetate in petrolether as eluent. White solid. Yield: 70 mg (45% of theory). Melting range: 209-213° C. HPLC (method 1): Rt=10.09 min. Mass spectroscopy: m/z: [M+H]+=447.0.

1. customThe reaction mixture was quenched with ammonium chloride solution
2. additiondiluted with water (20 mL)
3. extractionextracted with ethyl acetate (2×20 mL)
4. washThe organic layers were washed with brine
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customThe residue was purified by preparative TLC