HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → 3-Ethyl-3,5,5-trimethyl-1-(propan-2-yl)piperazin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Methyl Ethyl Ketone | HCID 6569 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Amino-1,1-dimethylethylisopropylamine | HCID 79532 | — |
| Product | 3-Ethyl-3,5,5-trimethyl-1-(propan-2-yl)piperazin-2-one | HCID 12580994 | 33% |
Reaction Steps
40 g (1 mol) of finely ground NaOH are added, with stirring, to a solution of 24.6 g (0.189 mol) of N-1-isopropyl-2-methylpropane-1,2-diamine (prepared in accordance with M. Senkus.: J. Am. Chem. Soc. 68, 10 (1946)) and 25 ml (0.3 mol) of chloroform in 250 ml (2.77 mol) of methyl ethyl ketone at 10° C. The reaction mixture is stirred for 16 hours at room temperature and is then filtered. The filtrate, concentrated by evaporation in a rotary evaporator, is chromatographed over silica gel with hexane/ethyl acetate (3:2). The pure fractions are concentrated by evaporation, giving 13.7 g (33%) of compound (229) in the form of a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06664353B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-5cad7f7b6ed0406aa96c01ded5c7288c |
| Source note | uspto-grants-2003_12 |