反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethyl 3-(4-fluoro-3-methoxyphenyl)propanoate (1.019 g, 4.50 mmol) was dissolved in THF (22.52 ml) under nitrogen. A solution of lithium aluminum hydride (4.50 ml, 9.01 mmol) was added slowly. TLC shows reaction done after about 10 min. Water (0.35 mL) was slowed added and then the mixture was stirred for 30 min. 1 N NaOH (1.05 mL) was added and the reaction was stirred for 30 min. Additional water was added (0.35 mL) and the solution was stirred and then filtered. The cake was washed with ether and then rotovapped. Ether was added. The solution was dried over magnesium sulfate and then filtered and rotovapped. The solution was passed through silica gel with methylene chloride then ethyl acetate then rotovapped to give 3-(4-fluoro-3-methoxyphenyl)propan-1-ol (0.753 g, 4.09 mmol, 91% yield) as a colorless oil: 1H NMR (400 MHz, CDCl3). δ ppm 6.98 (dd, 1H), 6.80 (dd, 1H), 6.71 (ddd, 1H), 3.89 (s, 3H), 3.68 (t, 2H), 2.68 (t, 2H), 1.94-1.82 (m, 2H), 1.33 (s, 1H)
reaction
the reaction was stirred for 30 min
the solution was stirred
filtered
The cake was washed with ether
Ether was added
The solution was dried over magnesium sulfate
filtered
来源 ID: ord-e9b1fdf073754fbab4f7c08378c9c1fc