HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N-Dimethylethylenediamine → Ammonium Hydroxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N-Dimethylethylenediamine | HCID 66053 | — |
| Reactant | 3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide | HCID 59212684 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ammonium Hydroxide | HCID 14923 | — |
| Product | 3-(8-(2,6-difluorophenyl)-2-{[2-(dimethylamino)ethyl]amino}-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl)-4-methyl-N-propylbenzamide | HCID 59212732 | — |
Reaction Steps
3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide (0.07 g, 0.13 mmol), N,N-dimethylethylenediamine (0.0173 g, 0.15 mmol), and TEA (0.026 g, 0.26 mmol) were combined in CH2Cl2 (5 mL) and stirred under argon at room temperature for 1 h. The solvents were pumped off in vacuo. The residue was flash chromatographed on silica gel (10 g) eluted with CH2Cl2 to 6:1:0.1, CH2Cl2:ethanol:NH4OH to give the title compound as a white amorphous solid. mp 139-142° C. LC-MS m/z 521 (M+H)+, 1.61 min (ret time).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354416B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-a9e5a50b16c043deae4bc307c4dd4e90 |
| Source note | uspto-grants-2013_01 |