反应详情

A mixture of 4-methoxycarbonyl-3-nitrobenzoic acid (2.25 g), 1M borane in tetrahydrofuran solution (50 ml) and dry tetrahydrofuran (45 ml) was stirred at room temperature for 48 hours. To this mixture, methanol (2 ml) and 1N hydrochloric acid (10 ml) were added and then the solvents were evaporated off. The crude residue was taken up with ethyl acetate, washed in turn with water and sat. sodium bicarbonate solution, dried over magnesium sulfate and evaporated to give an oil which was chromatographed on silica gel. Elution with toluene-chloroform (1:1) gave methyl 4-hydroxymethyl-2-nitrobenzoate (1.85 g).

1. customthe solvents were evaporated off
2. washwashed in turn with water and sat. sodium bicarbonate solution
3. dry with materialdried over magnesium sulfate
4. customevaporated
5. customto give an oil which
6. customwas chromatographed on silica gel
7. washElution with toluene-chloroform (1:1)