反应详情

温度

-50 °C

A solution of methyl 5-bromo-2-(2-thienylmethoxy)benzoate (1.6 g, 4.9 mmol) in dichloromethane (20 ml) was cooled to -85° C. A solution of DIBAL (5.8 ml, 1N in CH2Cl2) was added dropwise. The temperature was maintained below -75° C. for 30 minutes and then warmed to -50° C. over 21/2% hours. The reaction mixture was quenched with 1N HCl, washed with aqueous sodium hydrogen carbonate solution, dried (MgSO4) and evaporated. The product was purified by chromatography (eluant: diethyl ether/hexane) to give 5-bromo-2-(2-thienylmethoxy)benzyl alcohol a colourless gum (0.53 g, 36.4%).

1. temperatureThe temperature was maintained below -75° C. for 30 minutes
2. customThe reaction mixture was quenched with 1N HCl
3. washwashed with aqueous sodium hydrogen carbonate solution
4. dry with materialdried (MgSO4)
5. customevaporated
6. customThe product was purified by chromatography (eluant: diethyl ether/hexane)