反应详情

A solution of Intermediate 2 (111 mg, 0.569 mmol) in AcOH (15 ml) was passed through a Rh/C catalyst cartridge on an H-Cube hydrogenation apparatus at a pressure of 80 bar and a flow rate of 1 ml/min at 100° C. The reaction was looped through the apparatus for 2 h. The crude reaction mixture was concentrated and purified on 12 g SiO2 column with 0-10% NH3/MeOH CH2Cl2 to give the desired compound (90 mg, 80%). MS (ESI): mass calcd. for C12H13N3, 199.3. m/z found, 200.2 [M+H]+.

1. customat 100° C
2. customThe crude reaction mixture
3. concentrationwas concentrated
4. custompurified on 12 g SiO2 column with 0-10% NH3/MeOH CH2Cl2