Methane → HCID 20041374、化合物
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[NH:11][CH2:12][CH2:13][CH2:14][N:15]=2)=[CH:6][CH:5]=1)([O-])=O.[ClH:16].C>C(O)C>[ClH:16].[ClH:16].[NH:15]1[CH2:14][CH2:13][CH2:12][N:11]=[C:10]1[C:7]1[CH:8]=[CH:9][C:4]([NH2:1])=[CH:5][CH:6]=1参加物
5
実験手順
A solution of the product of Stage (i) (20.5 g) in ethanol (150 ml) containing 2N hydrochloric acid (150 ml) was stirred in the presence of 10% palladised charcoal (2.0 g) under an atmosphere of hydrogen, until uptake ceased. The suspension was filtered through a pad of `hyflo`, the pad was washed with 50% aqueous ethanol (200 ml) and the combined filtrates evaporated under reduced pressure. Crystallisation of the residue from methanol-isopropyl acetate [1:1] (300 ml) gave the title compound as a powder (23.7 g), m.p.>300°.
後処理
- filtrationThe suspension was filtered through a pad of `hyflo`, the pad
- washwas washed with 50% aqueous ethanol (200 ml)
- customthe combined filtrates evaporated under reduced pressure
- customCrystallisation of the residue from methanol-isopropyl acetate [1:1] (300 ml)
出典と根拠
- ORDレコード
- ord-cb4c452a90ef4bc8b6f65f8824f3ac21
- 出典データセット
- uspto-grants-1989_05
- 特許番号
- US04833153
反応ノート
読み込み中…