HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(4-(6-(2-Amino-5-bromonicotinoyl)pyridin-2-yl)-1,4-diazepan-1-yl)-3,3,3-trifluoropropan-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Carbodiimide | HCID 160435 | — |
| Reactant | 3,3,3-Trifluoropropionic acid | HCID 2777972 | — |
| Reactant | (6-(1,4-Diazepan-1-yl)pyridin-2-yl)(2-amino-5-bromopyridin-3-yl)methanone | HCID 24871523 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(4-(6-(2-Amino-5-bromonicotinoyl)pyridin-2-yl)-1,4-diazepan-1-yl)-3,3,3-trifluoropropan-1-one | HCID 24992834 | 54% |
Reaction Steps
(6-(1,4-diazepan-1-yl)pyridin-2-yl)(2-amino-5-bromopyridin-3-yl)methanone (650 mg, 1.36 mmol) was added to a stirred suspension of 3,3,3-trifluoropropionic acid (0.13 ml, 1.50 mmol), 1-hydroxybenzotriazole (184 mg, 1.36 mmol), triethylamine (1.33 ml, 9.52 mmol) and PS-carbodiimide (2.08 g, 2.72 mmol) in dichloromethane (20 ml). The resulting mixture was stirred at room temperature for 18 hours. The crude mixture was filtered and concentrated in vacuo. The residue was purified on silica gel by flash column chromatography (ISCO Companion|, 40 g column, 0-50% EtOAc/Petroleum ether) to afford the title compound as an orange solid (355 mg, 54% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188071B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-69b766f9079a42928d749c9e1d4ec367 |
| Source note | uspto-grants-2012_05 |