反应 #1914849

ord-c2042460c36e4b3cbb1553a6c5ff3a6a

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取The solution was then extracted with Et2O (2×100 mL)
  2. 2
    干燥dried (Na2SO4)
  3. 3
    过滤filtered
  4. 4
    浓缩concentrated in vacuo

实验过程

A solution of 3-chloro-5-methoxybenzaldehyde (22.8 g, 134 mmol; see step (i) above) in CH2Cl2 (250 mL) was cooled to 0° C. Boron tribromide (15.8 mL, 167 mmol) was added dropwise over 15 min. After stirring, the reaction mixture for 2 h, H2O (50 mL) was added slowly. The solution was then extracted with Et2O (2×100 mL). The organic layers were combined, dried (Na2SO4), filtered and concentrated in vacuo. Flash chromatography on silica gel eluting with Hex:EtOAc (4:1) afforded the sub-title compound (5.2 g, 25%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07056907B2uspto-grants-2006_06