反应详情

To a solution of the nitro compound 53 (256 mg, 0.57 mmol) in a mixture of MeOH (12 mL) and THF (4 mL) at 0° C. was added NiCl2.6H2O (279 mg, 1.14 mmol), followed by portion wise addition of NaBH4 (87 mg, 2.27 mmol). The reaction mixture turned black after 15 min, and was filtered through a celite pad; the filtrate concentrated under reduced pressure. The residue was suspended in 2N HCl and the solids were removed by filteration. The filtrate was basified with NH4OH to pH˜10 then extracted with EtOAc. The organic phase was concentrated to afford the title compound 54 (260 mg, crude, >100% yield, HPLC pure) as yellowish foam. MS (m/z): 420.1 (M+H).

1. filtrationwas filtered through a celite pad
2. concentrationthe filtrate concentrated under reduced pressure
3. customthe solids were removed by filteration
4. extractionthen extracted with EtOAc
5. concentrationThe organic phase was concentrated