反应详情

温度

0 °C

A solution of 2 g of sodium nitrite in 60 ml of water was added at 0° C. to a suspension prepared at 0° C. of 3.2 g of the product of Step A in 100 ml of concentrated hydrochloric acid and the mixture was stirred for 90 minutes at 0° C., then for one hour at 100° C. The cooled reaction mixture was poured into 100 ml of ice-cooled water and after separating and washing with water, the moist crude product was taken up in 100 ml of water, alkalinized with concentrated ammonium hydroxide, separated and washed with water to obtain after drying at 70° C., 1.47 g of the desired product melting at 180° C.

1. waitfor one hour at 100° C
2. customThe cooled reaction mixture
3. customafter separating
4. washwashing with water
5. customseparated
6. washwashed with water
7. customto obtain
8. customafter drying at 70° C.