HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium aluminum hydride → 6-[(3-Chloro-pyridin-4-ylmethyl)-amino]pyridin-3-yl-methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium aluminum hydride | HCID 28112 | — |
| Reactant | Sodium sulfate decahydrate | HCID 62649 | — |
| Reactant | 6-[(3-Chloro-pyridin-4-ylmethyl)-amino]-nicotinic acid methyl ester | HCID 57619295 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 6-[(3-Chloro-pyridin-4-ylmethyl)-amino]pyridin-3-yl-methanol | HCID 57619236 | 56% |
Reaction Steps
To 6-[(3-chloro-pyridin-4-ylmethyl)-amino]-nicotinic acid methyl ester (555, 1.00 g, 3.60 mmol) in tetrahydrofuran (120 mL) was added a solution of lithium tetrahydroaluminate (1.00 M in tetrahydrofuran, 5.00 mL) under an atmosphere of nitrogen at room temperature. The reaction was stirred at room temperature overnight, followed with addition of sodium sulfate decahydrate. After 1 hour, the reaction mixture was filtered, concentrated, and purified with silica gel column chromatography eluting with 2% to 20% methanol in dichloromethane to give the desired compound as a white solid (556, 0.5 g, 56%). MS (ESI) [M+H+]+=250.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461169B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-4f83570ff7744a7e806348b77c057886 |
| Source note | uspto-grants-2013_06 |