反応 #53429
ord-a00cbcb54b8f47ee845db3020a23743c
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他The reaction mixture is evaporated in vacuo
- 2その他the mixture is evaporated again
- 3抽出extracted several times with water
- 4その他The aqueous phase is evaporated to a very great extent
- 5その他an oil being obtained which
- 6その他crystallizes on standing
実験手順
3.0 g (16.4 mmol) of the compound from Example I are boiled under reflux for 17 hours in 250 ml of a saturated methanolic ammonia solution. The reaction mixture is evaporated in vacuo, the residue is taken up in methanol and the mixture is evaporated again; this process is repeated a few times. The crude product is taken up in dichloromethane and extracted several times with water. The aqueous phase is evaporated to a very great extent, an oil being obtained which crystallizes on standing.