HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 3-Bromo-7-(2-pyrrolidin-1-yl-ethyl)[1,5]naphthyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | (7-Bromo-1,5-naphthyridin-3-yl)acetaldehyde | HCID 21043926 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-Bromo-7-(2-pyrrolidin-1-yl-ethyl)[1,5]naphthyridine | HCID 10402869 | — |
Reaction Steps
To a stirred solution of the product from Example 153D (0.1 g, 0.4 mmol), acetic acid (0.4 mmol, 0.025 g) and pyrrolidine (0.44 mmol, 0.031 g) in dry THF (5 ml) NaBH(OAc)3 was added (0.6 mmol, 0.127 g). After 12 hr at room temperature the mixture was diluted with 50 mL of CH2Cl2 and washed successively with a saturated solution of sodium bicarbonate, brine and water. The organic layer was dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified over silica using 10% MeOH in CH2Cl2. The desired compound was obtained in 40%. 1H NMR (CDCl3, 300 MHz) δ 1.60 (m, 4H), 2.20 (m, 4H), 2.75 (m, 4H), 8.30 (m, 1H), 8.40 (m, 1H), 8.90 (m, 1H), 9.05 (m, 1H). MS (ESI) [M+H]+ at 307.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07456196B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-c3faa1c2c0c543ebba0d3033dcf48bee |
| Source note | uspto-grants-2008_11 |