反应详情

温度

5 °C

The product from step (e) (0.485 g) was suspended in conc.HCl (18 ml) which was then cooled to 15° C. A mixture of water (15 ml) and acetonitrile (25 ml) added to give a solution. Cooled to 5° C. and a solution of sodium nitrite (0.162 g) in water (1 ml) added drop-wise. Stirred at 5° C. for several hours then allowed to warm overnight. Solution cooled to −10° C. and neutralized with ammonia, then concentrated in vacuo. The yellow precipitate was collected by filtration and washed with water. Dried in vacuo to give 0.339 g of product. 67% yield.

1. additionadded
2. customto give a solution
3. temperatureto warm overnight
4. concentrationconcentrated in vacuo
5. filtrationThe yellow precipitate was collected by filtration
6. washwashed with water
7. customDried in vacuo