Methanol → 4-(3-amino-1H-pyrazol-1-yl)butan-1-ol
反応式
[N+:1]([C:4]1[CH:8]=[CH:7][N:6]([CH2:9][C:10]#[C:11][CH2:12][OH:13])[N:5]=1)([O-])=O.CO.NN>C(OCC)(=O)C.[Ni].O>[NH2:1][C:4]1[CH:8]=[CH:7][N:6]([CH2:9][CH2:10][CH2:11][CH2:12][OH:13])[N:5]=1参加物
7
実験手順
The 4-(3-nitro-pyrazol-1-yl)-but-2-yn-1-ol (prepared in example 52, 113 mg, 0.62 mmol) was dissolved in ethyl acetate (3 mL) and methanol (3 mL) was added. While stirring, a 50% slurry of raney nickel in water (1.3 mL) was added followed by hydrazine (400 μL). Immediate effervescence was observed. The reaction continued to stir and bubble for 25 min. The reaction was passed through a plug of celite and concentrated in vacuo to afford 4-(3-amino-pyrazol-1-yl)-butan-1-ol (93 mg, 98%) as a clear oil: ESI-LRMS m/e calcd for C7H13N3O [M+] 155.11, found 156.32 [M+H+].
後処理
- stirringto stir
- custombubble for 25 min
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-8148d61361804ced87872c86395c433e
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07935699B2
反応ノート
読み込み中…