HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclopentanecarbaldehyde → 1-(5-bromopyridin-3-yl)-N-(cyclopentylmethyl)methanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclopentanecarbaldehyde | HCID 70106 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 3-(Aminomethyl)-5-bromopyridine | HCID 22992264 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-(5-bromopyridin-3-yl)-N-(cyclopentylmethyl)methanamine | HCID 86698327 | 79.3% |
Reaction Steps
A solution of (5-bromopyridin-3-yl)methanamine (LVIII) (1.30 g, 5.8 mmol, 1.0 eq), cyclopentanecarbaldehyde (0.57 g, 5.8 mmol, 1.0 eq) and TEA (0.60 g, 5.8 mmol, 1.0 eq) in MeOH (15 mL) was stirred at room temperature for 2 h. Then NaBH3CN (1.98 g, 34.6 mmol, 6.0 eq) was added and the mixture was stirred at the same temperature for another 3 h. The solvent was removed under reduced pressure and the residue was diluted in water (20 mL) and extracted with DCM (10 mL×3), combined organic layers were dried over MgSO4 and concentrated in vacuo to give 1-(5-bromopyridin-3-yl)-N-(cyclopentylmethyl)methanamine (LIX) (1.23 g, 4.57 mmol, 79.3% yield) as a brown oil. ESIMS found for C12H17BrN2 m/z 269 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09233104B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-df0c51f3fedc4b8d9030010d8d80bc27 |
| Source note | uspto-grants-2016_01 |