反应详情

温度

0 °C

To a solution of 2-amino-6-chloropyridine (3.0 g, 23.3 mmol) in dichloromethane (45 mL) under argon was added triethylamine (4.10 mL, 29.2 mmol) and the reaction cooled to 0° C. (ice bath). A solution of trimethylacetyl chloride (3.16 mL, 25.7 mmol) in dichloromethane (10 mL) was added dropwise over 20 min before stirring for 30 min at 0° C. The reaction was brought up to rt and stirred for a further 5 h, then water (30 mL) was added. The organics were separated and washed with Na2CO3 solution (2×50 mL), dried,(MgSO4) and solvent removed in vacuo. Purification by column chromatography (SiO2, CH2Cl2) gave the title compound. m/z (ES+)=213.04 [M+H]+.

1. customwas brought up to rt
2. stirringstirred for a further 5 h
3. customThe organics were separated
4. washwashed with Na2CO3 solution (2×50 mL), dried,(MgSO4) and solvent
5. customremoved in vacuo
6. customPurification by column chromatography (SiO2, CH2Cl2)