HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → N-ethyl-4-methyl-3-(1-methylphthalazin-6-yl)benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 4-Methyl-3-(1-methylphthalazin-6-yl)benzoic acid | HCID 59726022 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | N-ethyl-4-methyl-3-(1-methylphthalazin-6-yl)benzamide | HCID 59726016 | — |
Reaction Steps
Into a 15-ml round-bottom flask were added 4-methyl-3-(1-methylphthalazin-6-yl)benzoic acid (51 mg, 183 μmol), hatu (105 mg, 275 μmol), ethylamine (2M solution in THF (275 μl, 550 μmol), and chloroform (1000 μl). 0.5 ml of N,N-Dimethylformamide was next added to the mixture, and the resulting golden yellow solution was stirred at RT for 3 h, during which LC-MS indicated completion of reaction. The reaction mixture was diluted with EtOAc and washed with water and brine, dried over MgSO4, filtered, and concentrated in vacuo. CombiFlash purification (1% to 5% MeOH/CH2Cl2) afforded the title compound (26) as a tan amorphous solid. MS (ES+): 306.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101612B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-e67aa7034d8f46d5a5ff3faf92c138df |
| Source note | uspto-grants-2012_01 |