反应详情

3 g of 1C was added to an ice-cold solution of 50% aqueous sulfuric acid, and the mixture maintained below 10° C. during the addition of a solution of 0.7 g of sodium nitrite in 10 ml of water. This mixture was then stirred for 1 hour, allowed to reach ambient temperature, and then extracted with ether. The organic layer was separated, solvent removed and the resulting red oil chromatographically purified and recrystallized to yield 1, as a crystalline solid, m.p.: 72°-73° C.

1. customto reach ambient temperature
2. extractionextracted with ether
3. customThe organic layer was separated
4. customsolvent removed
5. customthe resulting red oil chromatographically purified
6. customrecrystallized
7. customto yield 1