反应详情

Sodium metal was added portionwise to a solution of the product of example 32 step a) (5.0 g) in ammonia (150 ml) until a blue colouration persisted. Ammonium chloride was then added and the solvent allowed to evaporate. The residue was dissolved in H2O (200 ml) and filtered before neutralising with 2M HCl solution. The grey precipitate was filtered, washed with H2O (200 ml) and dried in vacuo for 48 h to yield the subtitle compound as a brown solid (3.0 g).

1. customto evaporate
2. dissolutionThe residue was dissolved in H2O (200 ml)
3. filtrationfiltered
4. filtrationThe grey precipitate was filtered
5. washwashed with H2O (200 ml)
6. customdried in vacuo for 48 h