HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl phenylmalonate → HCID 178429823, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl phenylmalonate | HCID 66514 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 5-methyl-1H-imidazol-2-amine | HCID 322559 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178429823 | HCID 178429823 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
18 g (135 mmol) 5-Methyl-1H-imidazol-2-ylamine are dissolved in 155 mL DMF and 31.8 g (135 mmol) diethyl phenylmalonate are added. After dropwise addition of 61.5 g (404 mmol) 1,8-diazabicyclo[5.4.0]undec-7-ene the reaction mixture is stirred at 100° C. for 16 h. The DMF has been removed and the darkbrown oily residue treated with 150 mL water (complete dissolution). 2M HCl (250 mL) is added at room temperature until a pH of 1. After stirring for 1 h at ice bath cooling the formed crystals are collected by filtration to yield the product (10.2 g=31%), which is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957064B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-0fdf9dfa638a4654b04b0bfb422ee590 |
| Source note | uspto-grants-2015_02 |