Methane → HCID 59300179、化合物
反応式
[N+:1]([C:4]1[CH:18]=[CH:17][C:7]([CH2:8][N:9]2[CH2:13][CH2:12][CH2:11][CH:10]2[CH:14]([OH:16])[CH3:15])=[CH:6][CH:5]=1)([O-])=O.C.O.NN>CO>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([CH2:8][N:9]2[CH2:13][CH2:12][CH2:11][CH:10]2[CH:14]([OH:16])[CH3:15])=[CH:17][CH:18]=1参加物
5
実験手順
1-[1-(4-Nitro-benzyl)-pyrrolidin-2-yl]-ethanol (370 mg, 1.48 mmol) is dissolved in MeOH (15 mL), to this solution is added FeCl3.6H2O (30 mg, 0.11 mmol) and active charcoal (15 mg, 1.2 mmol). The suspension is heated to reflux. Hydrazine hydrate (1.0 mL) is added, and reflux is continued for 3 h. After the mixture is cooled to room temperature, the active charcoal is filtered off through Celite, and the MeOH is removed under reduced pressure. The residue (200 mg, 61%) is directly used in the next step.
後処理
- temperatureThe suspension is heated to reflux
- temperaturereflux
- filtrationthe active charcoal is filtered off through Celite
- customthe MeOH is removed under reduced pressure
出典と根拠
- ORDレコード
- ord-96cfde47a6064f90956192de1e8bea49
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07713994B2
反応ノート
読み込み中…