Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 10740435 | HCID 10740435 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10093635 | HCID 10093635 | 77.1% |
Reaction Steps
1.50 g (3.63 mmol) of Compound 159 obtained in EXAMPLE 159 was dissolved in 30 mL of dimethylformamide, 1.48 g (18.2 mmol) of dimethylamine hydrochloride and 2.50 g (18.2 mmol) of potassium carbonate were added, and the mixture was stirred at 50° C. for 30 minutes. Water was added to the reaction solution and the mixture was extracted with ethyl acetate. The organic layer was washed with water and an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane, to give 1.18 g of Compound 161 (yield: 77%). This compound was dissolved in ethyl acetate, 3 mL of a 1N hydrochloric acid/2-propanol solution was added, and the precipitated crystals were collected by filtration, to give a hydrochloride of Compound 161.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05539112 |
|---|
| Source dataset | uspto-grants-1996_07 |
|---|
| ORD ID | ord-169470d914574346a18899fbad40d767 |
|---|
| Source note | uspto-grants-1996_07 |
|---|