HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N'-Dimethylethylenediamine → HCID 123141395, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| Reactant | 2-Pyrrolidone | HCID 12025 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 123606779 | HCID 123606779 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 123141395 | HCID 123141395 | 89.3% |
Reaction Steps
The compound (650 mg, 1.00 mmol) of Example 293, step A, 2-pyrrolidone (128 mg, 1.50 mmol), copper iodide(I) (19 mg, 0.10 mmol), N,N′-dimethylethylenediamine (0.022 ml, 0.20 mmol) and potassium phosphate (425 mg, 2.00 mmol) were dissolved in toluene (4.0 ml), and the mixture was heated under reflux for 7 hr. The reaction mixture was diluted with ethyl acetate and water, and the organic layer was extracted. The organic layer was washed with saturated brine and dried over sodium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure. The obtained oil was purified by silica gel column chromatography (ethyl acetate-hexane) to give the title compound (542 mg, yield 89%) as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513235B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-1ad1d2c1dafc48f781bb2071322228a4 |
| Source note | uspto-grants-2013_08 |