HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 4-((7-Chlorothieno[3,2-b]pyridin-2-yl)methyl)morpholine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 7-Chlorothieno[3,2-b]pyridine-2-carbaldehyde | HCID 50988849 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethylacetate methanol | HCID 21584119 | — |
| Product | 4-((7-Chlorothieno[3,2-b]pyridin-2-yl)methyl)morpholine | HCID 59424692 | 29.4% |
Reaction Steps
To a solution of aldehyde 14 (scheme 3) (316 mg, 1.6 mmol) and morpholine (0.15 ml, 1.52 mmol) in MeOH (20 mL) was added acetic acid (0.88 ml, 15 mmol), followed by sodium cyanoborohydride (105 mg, 1.67 mmol). The resultant mixture was allowed to stir for 18 h, quenched with saturated aqueous potassium carbonate solution (5 mL), evaporated under reduced pressure and the residue was partitioned between EtOAc and water. The organic phase was dried over anhydrous sodium sulfate, concentrated to dryness and the remained solid was purified by column chromatography, eluents EtOAc/hexane (30:70), then MeOH/EtOAc (1:99), to afford the title compound 131 (120 mg, 29% yield). MS (m/z) 269.0/271.0 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07772247B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-8571b762a51641a9ba3d9c4b8fac5a3a |
| Source note | uspto-grants-2010_08 |