反应详情

温度

-40 °C

Compound 29 (1.8 g, 5.44 mmol) was transferred to a flame-dried flask filled with argon and dissolved in anhydrous THF then cooled to −40° C. Triethylamine (0.72 g, 7.07 mmol) was added by syringe followed by MeSO2Cl (0.75 g, 6.53 mmol). The temperature of the reaction mixture was allowed to rise to room temperature (10-15 minutes) before it was quickly filtrated and concentrated. The crude oil was dissolved in CH2Cl2 and washed with H2O. The organic phase was dried with MgSO4, filtrated and concentrated in vacuo to a dark, brown oil. The crude product was used immediately in the next step.

1. additionfilled with argon
2. customto rise to room temperature
3. custom(10-15 minutes)
4. filtrationwas quickly filtrated
5. concentrationconcentrated
6. dissolutionThe crude oil was dissolved in CH2Cl2
7. washwashed with H2O
8. dry with materialThe organic phase was dried with MgSO4
9. filtrationfiltrated
10. concentrationconcentrated in vacuo to a dark, brown oil