HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 18472328, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diethyl cyanophosphonate | HCID 76257 | — |
| Reactant | (4-Amino-benzyl)-methyl-(tetrahydro-pyran-4-yl)-amine | HCID 9877845 | — |
| Reactant | HCID 18472593 | HCID 18472593 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18472328 | HCID 18472328 | 23.5% |
Reaction Steps
To a solution of 7—(3-pyridyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (0.15 g), 4—(N-methyl-N-(tetra-hydropyran-4-yl)aminomethyl)aniline (0.12 g) and triethylamine (0.16 ml) in dimethylformamide (50 ml) was added diethyl cyano-phosphate (0.1 ml) under ice-cooling, and the mixture was stirred under nitrogen atmosphere at room temperature over night. The solvent was evaporated, and the residue was purified with silica gel column (methanol/ethyl acetate/triethylamine) to give crude crystals, which were recrystallized from ethanol-hexane to give 7—(3-pyridyl)-N-(4—((N-tetrahydropyran-4-yl-N-methylamino)-methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (Compound 146) (0.06 g) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06413947B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-9e5b7d35cf3e48e19a5ffdc61ff51021 |
| Source note | uspto-grants-2002_07 |