反应详情

TFA (0.5 mL) was added to compound 12d) (170 mg, 0.311 mmol) in dichloromethane (5 mL) at room temperature and the solution was stirred for 2 h. The reaction mixture was then diluted with water, adjusted to pH 8 via addition of saturated sodium hydrogen carbonate solution and extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and evaporated. The remnant was purified by preparative TLC using a blend of 5% methanol in dichloromethane as eluent. White solid. Yield: 75 mg (51% of theory). Melting range: 193-197° C. HPLC (method 3): Rt=4.02 min. Mass spectroscopy: m/z: [M+H]+=446.1.

1. extractionextracted with dichloromethane
2. dry with materialThe combined organic layers were dried over sodium sulfate
3. customevaporated
4. customThe remnant was purified by preparative TLC