HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66707062, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Reactant | HCID 57656359 | HCID 57656359 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66707062 | HCID 66707062 | 93% |
Reaction Steps
Combine 3-(tert-butoxycarbonyl)-6-(4-carboxy-benzylamino)-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.1 g, 0.3 mmol), methylamine hydrochloride (31 mg, 0.46 mmol), triethylamine (0.1 g, 0.9 mmol), HATU (0.2 g, 0.5 mmol), anhydrous DMF (3 mL) and stir at ambient temperature for 17 h. Partition the reaction mixture between brine (5 mL) and diethyl ether (5 mL), separate the organic layer and dry over anhydrous Na2SO4. Evaporate the solvent to obtain 3-(tert-butoxycarbonyl)-7-chloro-6-(4-methylcarbamoyl-benzylamino)-2,3,4,5-tetrahydro-1H-benzo[d]azepine as a yellow oil (0.1 g, 93%). MS (ES+) m/z: 344 (M+H−Boc)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-29d5ea49dca94a2ea6c7f72dbb475bcf |
| Source note | uspto-grants-2011_09 |