HCID 21951129、化合物 → N1-(2-Hydroxyethyl)-2-methyl-1,2-propanediamine
反応式
[CH3:1][C:2]([N+:9]([O-])=O)([CH3:8])[CH2:3][NH:4][CH2:5][CH2:6][OH:7]>CO.[Ni].O>[NH2:9][C:2]([CH3:8])([CH3:1])[CH2:3][NH:4][CH2:5][CH2:6][OH:7]参加物
5
実験手順
To a solution of 2-((2-methyl-2-nitropropyl)amino)ethanol (20.4 g, 126 mmol) in methanol (120 ml) was added a slurry of 50% Raney Nickel® in H2O (6 ml). The vessel was pressurized with H2 (450 psi) and the suspension stirred for 19 h. The mixture was filtered through Celite and concentrated in vacuo to give 20 g of a crude liquid, which was distilled under vacuum (<1 mbar, 100-125° C.) to give 13 g of a clear liquid, which was found to be partially purified and was used directly in the next step without purification. LRMS (ESI/APCI) m/z 133 [M+H]+.
後処理
- filtrationThe mixture was filtered through Celite
- concentrationconcentrated in vacuo
- customto give 20 g of a crude liquid, which
- distillationwas distilled under vacuum (<1 mbar, 100-125° C.)
出典と根拠
- ORDレコード
- ord-e79538a208514dc2bab55a69f72a986c
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09248117B2
反応ノート
読み込み中…