反应详情

温度

0 °C

Sodium methoxide (0.30 g) was added to a solution of the product from step (d) (1.5 g) in DMF (15 ml) at 0° C. To the resulting solution was added dropwise a suspension of paraformaldehyde (0.19 g) in DMF (20 ml). The resulting mixture was stirred at 0° C. for 1.5 hours, then poured into water and extracted with ethyl acetate. The combined extracts were washed with water and brine, dried and evaporated in vacuo to give a yellow oil which was eluted through a silica column using DCM/EtOH/NH4OH (50:8:1) as eluant to give the desired product as an off-white solid (0.85 g) which was recrystallised from ethanol.

1. additionTo the resulting solution was added dropwise
2. extractionextracted with ethyl acetate
3. washThe combined extracts were washed with water and brine
4. customdried
5. customevaporated in vacuo
6. customto give a yellow oil which
7. washwas eluted through a silica column