反应详情

温度

72.5 °C

A mixture of compound 16 (100 mg), paraformaldehyde (110 mg), p-toluenesulfonic acid (60 mg) in benzene (5 mL) was stirred at 70-75° C. for 14 h. The reaction solution was filtrated, washed with sat. NaHCO3 and concentrated to give crude title product 17 in an estimated yield of ˜50% by TLC and NMR. Chromatography on SiO2 (CH2Cl2/EtOAc 10:1) provided pure sample for confirmation of the structure.

1. filtrationThe reaction solution was filtrated
2. washwashed with sat. NaHCO3
3. concentrationconcentrated
4. customto give crude title product 17 in an estimated yield of ˜50% by TLC and NMR
5. customChromatography on SiO2 (CH2Cl2/EtOAc 10:1) provided pure sample for confirmation of the structure