HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23158224, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| Reactant | Methyl 2,6-dimethoxynicotinate | HCID 10703069 | — |
| Reactant | Triethylaluminum | HCID 16682930 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 23158224 | HCID 23158224 | — |
Reaction Steps
Under nitrogen atmosphere, 15% hexane solution of triethyl aluminium was dropped at 0° C. to 26 m solution of toluene with 0.6 ml of N,N′-dimethyl-ethan-1,2-diamine, and the mixture was stirred at room temperature for 1 hour. Then, 5 ml solution of toluene with 1 g of 2,6-dimethoxy-nicotinic acid methylester was dropped at room temperature, and the mixture was stirred at 130° C. for 1 hour. The reaction solution was cooled down under ice temperature, 1M of hydrochloric acid was added, and extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure to obtain 156 mg of the above compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07902369B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-ada68284eabd4dc8a978ddba728bc826 |
| Source note | uspto-grants-2011_03 |