反应详情

温度

45 °C

A solution of crude 8-bromo-N-(2-chlorophenyl)-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carbohydrazonamide (195, 0.434) in methanol (5 mL) was treated with a solution of cyanogen bromide (115 mg, 1.1 mmol) in methanol (1 mL) at room temperature. The reaction vessel was sealed and heated at 45° C. for 2 h, cooled to room temperature, quenched upon addition of saturated sodium bicarbonate and extracted with ethylacetate. The combined organics were dried over sodium sulfate and concentrated and the residue purified by flash column chromatography (1-10% MeOH in methylene chloride to give 287 (43 mg, 21% yield). MS (ESI): 475.0

1. customThe reaction vessel was sealed
2. temperaturecooled to room temperature
3. customquenched upon addition of saturated sodium bicarbonate
4. extractionextracted with ethylacetate
5. dry with materialThe combined organics were dried over sodium sulfate
6. concentrationconcentrated
7. customthe residue purified by flash column chromatography (1-10% MeOH in methylene chloride