反应 #1563923

ord-2589af82d320479285015e66f2b33f07

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heat to 65° C.
  2. 2
    workup.STIRRINGstir for 4 h
  3. 3
    浓缩Concentrate the mixture under reduced pressure

实验过程

Dissolve 1-(2,2-dimethoxyethoxy)-4-fluorobenzene (1.00 g, 4.99 mmol) in chloroform (5.0 mL) and treat the mixture with trifluoroacetic acid (0.755 mL, 9.99 mmol). Stir the mixture at room temperature for two days, then heat to 65° C. and stir for 4 h. Concentrate the mixture under reduced pressure to furnish the title compound as a colorless oil in ca. 70% purity, as indicated by 1H NMR analysis (550 mg, 71% uncorrected yield). 1H NMR (400 MHz, CDCl3): δ 9.85 (t, J=0.5 Hz, 1H), 7.00 (dd, J=8.9, 8.5 Hz, 2H), 6.85 (dd, J=9.5, 4.3 Hz, 2H), 4.55 (br s, 2H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09402838B2uspto-grants-2016_08