HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl 5-aminopyridine-3-carboxylate → (5-Aminopyridin-3-yl)methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl 5-aminopyridine-3-carboxylate | HCID 1514432 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (5-Aminopyridin-3-yl)methanol | HCID 29921874 | — |
Reaction Steps
5-Amino-nicotinic acid methyl ester (5.7 g, 30.2 mmol) was dissolved in THF (150 ml) and LiAlH4 (1M in THF solution 133 ml, 133 mmol) added slowly at 0° C. The reaction mixture was stirred at room temperature for 21 h. The reaction mixture was quenched and acidified to pH 3 using dilute HCl, and basified (pH 8) using solid Na2CO3. Solvents were removed under reduced pressure. The residue was filtered through silica gel using 20% MeOH/DCM yielding the product 3.8 g, (100%) with LCMS purity 97%, m/z 125 [M++H]+, by ELS.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939666B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-aba6cc03212c405e89b4b5713114bf63 |
| Source note | uspto-grants-2011_05 |