反应详情

A 500 mL Parr bottle was flushed with argon, then 3-isopropoxybenzonitrile (32 g, 198 mmol) was added and diluted with 150 mL EtOH. The reaction was charged with ˜2 mL of an aq. slurry of Raney Nickel, then affixed to a Parr hydrogenation apparatus. The flask was evacuated and flushed with N2 three times before being charged with 40 psi H2. The flask was allowed to shake for 3 hr over which time the flask was recharged to 40 psi and consumption of gas ceased. HPLC/MS showed no starting material so the catalyst was carefully filtered without drying and washed with EtOH. The filtrate was concentrated and purified on an Isco automated system affixed with a Biotage Flash 40(M) cartridge eluted with 0-5% (MeOH+0.5M NH3) in CH2Cl2 over 30 min at 40 mL/min to give the product.

1. customA 500 mL Parr bottle was flushed with argon
2. customThe flask was evacuated
3. customflushed with N2 three times
4. additionbefore being charged with 40 psi H2
5. customthe flask was recharged to 40 psi and consumption of gas
6. filtrationwas carefully filtered
7. customwithout drying
8. washwashed with EtOH
9. concentrationThe filtrate was concentrated
10. custompurified on an Isco automated system
11. washeluted with 0-5% (MeOH+0.5M NH3) in CH2Cl2 over 30 min at 40 mL/min
12. customto give the product