反应详情

温度

0 °C

To a solution of Intermediate 97a (187 mg, 0.288 mmol) and DIPEA (0.151 mL, 0.865 mmol) in DCM (5 mL) at 0° C. was added mesyl chloride (0.056 mL, 0.721 mmol) and the resulting orange solution stirred at 0° C. for 1 h. Water (5 mL) was added and the mixture shaken. The aqueous layer was extracted with DCM (5 mL), then the combined organics passed through a hydrophobic fit and concentrated in vacuo to leave the mixture of title compounds as a brown gum. LCMS (Method 4): 1:1 ratio, Rt 3.87 min, m/z 727 [MH+] and Rt 4.11, m/z 667 [MH+].

1. stirringthe mixture shaken
2. extractionThe aqueous layer was extracted with DCM (5 mL)
3. concentrationconcentrated in vacuo
4. customto leave
5. additionthe mixture of title compounds as a brown gum