HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 6-chloro-N-(propan-2-yl)pyridin-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetone | HCID 180 | — |
| Reactant | 5-Amino-2-chloropyridine | HCID 79305 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | 6-chloro-N-(propan-2-yl)pyridin-3-amine | HCID 58957920 | 76.3% |
Reaction Steps
To a solution of 2-chloro-5-aminopyridine (500 mg, 3.88 mmol) and acetone (250 μL, 4.27 mmol) in dichloroethane (13 mL) was added NaBH(OAc)3 (989 mg, 4.66 mmol) and AcOH (330 μL, 5.82 mmol). The reaction was stirred for 24 hours and was diluted with 1N NaOH. The aqueous solution was washed with CH2Cl2 (3×). The combined organic solutions were dried (Na2SO4), filtered and concentrated. Purification by medium pressure chromatography eluting with a solvent gradient (2% MeOH in CH2Cl2 to 5% MeOH in CH2Cl2) provided 505.2 mg of (6-chloro-pyridin-3-yl)-isopropyl-amine. 1H NMR (CD3OD) δ 7.64 (d, 1H), 7.10 (d, 1H), 6.99 (dd, 1H), 3.55 (m, 1H), 1.17 (d, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07358242B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-50d4216d633041dd8a004bdefe328e0e |
| Source note | uspto-grants-2008_04 |