反应详情

温度

200 °C

Compound N-(2,5-dichloro-pyridin-4-ylmethyl)-acetamide (250 mg, 1.14 mmol) was added to 33% H2SO4 (3 mL) and the mixture heated in a CEM microwave reactor at 200° C. for 30 min. After cooling to room temperature, the reaction mixture was diluted with water (20 mL) and basified with excess concentrated NH4OH. The reaction mixture was then frozen using a dry ice/acetone bath and evaporated to dryness in vacuo overnight in a freeze-dry apparatus. The solids were purified by column chromatography using a 12 g ISCO combi-flash column and dry-loading cartridge (silica gel, 100:0 to 50:50 DCM:DCM/MeOH/NH4OH 6:3:1) to afford N-(5-chloro-2-oxo-1,2-dihydro-pyridin-4-ylmethyl)-acetamide (246 mg, quant.) as an off-white solid. This material was directly in the next step.

1. temperatureAfter cooling to room temperature
2. temperatureThe reaction mixture was then frozen
3. customevaporated to dryness in vacuo overnight in a freeze-dry apparatus
4. customThe solids were purified by column chromatography
5. dry with materialdry-loading cartridge (silica gel, 100:0 to 50:50 DCM:DCM/MeOH/NH4OH 6:3:1)