反应详情

温度

0 °C

Dichloromethane (200 mL) and diisopropylethylamine (2 g, 17.16 mmol) were added to the product of step (vii) (4 g, 11.46 mmol). The resulting solution was cooled to 0° C. and MsCl (2 g, 17.16 mmol) added dropwise. When the addition was completed, the resulting solution was stirred at 0° C. for 10 minutes and at room temperature for 2 hours. The reaction mixture was extracted with dichloromethane and washed with water (×3). The combined organic extract was dried over MgSO4, filtered and concentrated in vacuo, which afforded the subtitle compound (viii) as a yellow brown solid (4.5 g).

1. additionWhen the addition
2. extractionThe reaction mixture was extracted with dichloromethane
3. washwashed with water (×3)
4. extractionThe combined organic extract
5. dry with materialwas dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo, which