反应详情

温度

0 °C

To solution of Intermediate 2A (2.2 g, 5.2 mmol) in THF (50 mL) cooled to 0° C. was added TBAF (6.3 mL, 6.3 mmol) via dropwise addition. The reaction mixture was stirred at 0° C. for 1 h, then diluted with ethyl acetate (200 mL). The organic layer was washed with water (2×100 mL), dried over Na2SO4 and dried in vacuo. The product was purified by silica gel chromatography (80 g silica gel; linear gradient 0-25% ethyl acetate for 30 min) to obtain 917 mg (97% yield) of Intermediate 2B. HPLC/MS (Method D) RT=1.00 min, [M−H2O+1]+ 199.1.

1. additionvia dropwise addition
2. washThe organic layer was washed with water (2×100 mL)
3. dry with materialdried over Na2SO4
4. customdried in vacuo
5. customThe product was purified by silica gel chromatography (80 g silica gel; linear gradient 0-25% ethyl acetate for 30 min)