反应 #481600

ord-2c30a265a15946deb2c3af6cb2cd1968

反应方程式

COc1cc(C=O)cc(OC)c1OC
3,4,5-trimethoxy benzaldehyde
O=S(=O)(O)O
sulphuric acid
COc1cc(C=O)cc(OC)c1O
3,5-Dimethoxy-4-hydroxy benzaldehyde

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他at 40° C.
  2. 2
    其他for 8 hours

实验过程

Monodemethylation of 3,4,5-trimethoxy benzaldehyde using sulphuric acid at 40° C. for 8 hours yields 3,5-Dimethoxy-4-hydroxy benzaldehyde (Syringaldehyde). Condensation of syringaldehyde with ethyl cyanoacetate in the presence of piperidine—acetic acid and benzene as the reaction medium at reflux temperature under continuous azeotropic water removal yields the title product. The reaction takes about 1.5 hours for completion. The yield obtained is typically 95%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06602515B2uspto-grants-2003_08