反应 #45919

ord-803d65da74664f0e8ad0f65cc171b8de

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling to rt
  2. 2
    其他the reaction was quenched by cold H2O (50 mL)
  3. 3
    萃取the resulting mixture was extracted with EtOAc (3×100 mL)
  4. 4
    洗涤The combined EtOAc extracts were washed with brine (3×50 mL)
  5. 5
    干燥dried (anhydrous Na2SO4)
  6. 6
    其他The solvent was removed in vacuo

实验过程

To a stirred solution of 3-hydroxybenzaldehyde (20 mmol) in DMSO (50 mL) at rt, solid Cs2CO3 (60 mmol) was added. 1-(2-chloroethyl)pyrrolidine hydrochloride (30 mmol) was added to the reaction mixture and heated to 90° C. for 9 h. After cooling to rt, the reaction was quenched by cold H2O (50 mL), and the resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine (3×50 mL) and dried (anhydrous Na2SO4). The solvent was removed in vacuo to afford crude 3-(2-pyrrolidin-1-yl-ethoxy)benzaldehyde.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737285B2uspto-grants-2010_06