HCID 21951129, 화합물 → N1-(2-Hydroxyethyl)-2-methyl-1,2-propanediamine
반응식
[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]참가 물질
5
실험 절차
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]+.
후처리
- 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.)
출처 및 근거
- ORD 기록
- ord-e79538a208514dc2bab55a69f72a986c
- 출처 데이터셋
- uspto-grants-2016_02
- 특허 번호
- US09248117B2
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