HCID 21951129, compound → N1-(2-Hydroxyethyl)-2-methyl-1,2-propanediamine

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]+.

1. filtrationThe mixture was filtered through Celite
2. concentrationconcentrated in vacuo
3. customto give 20 g of a crude liquid, which
4. distillationwas distilled under vacuum (<1 mbar, 100-125° C.)

ORD record

ord-e79538a208514dc2bab55a69f72a986c

Source dataset

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09248117B2