2-Imidazolidinone → HCID 21453127, compound
Reaction equation
[NH:1]1[CH2:5][CH2:4][NH:3][C:2]1=[O:6].[C:7](Cl)(=[O:12])[C:8]([CH3:11])([CH3:10])[CH3:9].C(N(CC)CC)C>O1CCCC1>[C:7]([N:1]1[CH2:5][CH2:4][NH:3][C:2]1=[O:6])(=[O:12])[C:8]([CH3:11])([CH3:10])[CH3:9]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
A suspension, cooled to 0° C, of imidazolidin-2-one (17.2 parts by weight) in tetrahydrofurane (200 parts by volume) was treated dropwise over the course of one hour, with pivaloyl chloride (24.2 parts by weight) at the same temperature. The mixture was then stirred for a further 3 hours at 0° C, triethylamine (27.8 parts by volume) was subsequently added dropwise while cooling with ice water, and the mixture was then left to stand overnight at room temperature. The triethylamine hydrochloride which had separated out was then filtered off, the filtrate was completely concentrated in vacuo by means of a rotary evaporator and the residue was further warmed for 1 hour, in vacuo, in a bath at 60° C. The oily product (crude yeild: 32.8 parts by weight) was further processed, as it was. When an attempt was made to distill the substance in vacuo, severe decomposition occurred.
Workup
- waitthe mixture was then left
- waitto stand overnight at room temperature
- customThe triethylamine hydrochloride which had separated out
- filtrationwas then filtered off
- concentrationthe filtrate was completely concentrated in vacuo by means of a rotary evaporator
- temperaturethe residue was further warmed for 1 hour, in vacuo, in a bath at 60° C
- distillationto distill the substance in vacuo, severe decomposition
Sources & evidence
- ORD record
- ord-9768e4fdc1e04982be2388db72d9597c
- Source dataset
- uspto-grants-1977_02
- Patent number
- US04009272
Reaction notes
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