反应 #1563923
ord-2589af82d320479285015e66f2b33f07
反应方程式
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度heat to 65° C.
- 2workup.STIRRINGstir for 4 h
- 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).