反应详情

温度

110 °C

Add dry toluene (6.06 mL) to a mixture of 2,9-dimethyl-1,10-phenanthroline (76.52 mg), copper(I) iodide (69.27 mg), sodium tert-butoxide (475.59 mg), 4-mercapto-piperidine-1-carboxylic acid tert-butyl ester (583.5 mg), magnesium (49.10 mg) and 2-amino-5-iodopyridine (550 mg). Bubble nitrogen into the mixture with ultrasound and stir the suspension at 110° C. in a sealed tube for 24 h. Cool and filter through celite. Wash with toluene and remove the solvent under vacuum. Add hexane/EA (1/1) and filter through a celite/silica gel pad, washing twice with hexane/EA (1/1) and then EA. Remove the solvent under vacuum. Purify by silica gel column chromatography eluting with hexane/EA (50-75%) to afford 630 mg of the title compound. MS (ES+): m/z=310 (M+H)+

1. temperatureCool
2. filtrationfilter through celite
3. washWash with toluene
4. customremove the solvent under vacuum
5. filtrationAdd hexane/EA (1/1) and filter through a celite/silica gel pad
6. washwashing twice with hexane/EA (1/1)
7. customRemove the solvent under vacuum
8. customPurify by silica gel column chromatography
9. washeluting with hexane/EA (50-75%)